CN103179943A - Hair-mending compositions and associated methods - Google Patents

Hair-mending compositions and associated methods Download PDF

Info

Publication number
CN103179943A
CN103179943A CN2011800510808A CN201180051080A CN103179943A CN 103179943 A CN103179943 A CN 103179943A CN 2011800510808 A CN2011800510808 A CN 2011800510808A CN 201180051080 A CN201180051080 A CN 201180051080A CN 103179943 A CN103179943 A CN 103179943A
Authority
CN
China
Prior art keywords
compositions
hair
approximately
pec
batch
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2011800510808A
Other languages
Chinese (zh)
Other versions
CN103179943B (en
Inventor
M·赖特
M·斯泽曾
J·科恩
D·佩特罗斯基
D·伊根
C·菲尔斯基
G·M·维布姆
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Alberto Culver Co
Original Assignee
Alberto Culver Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Alberto Culver Co filed Critical Alberto Culver Co
Publication of CN103179943A publication Critical patent/CN103179943A/en
Application granted granted Critical
Publication of CN103179943B publication Critical patent/CN103179943B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/342Alcohols having more than seven atoms in an unbroken chain
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • A61K8/375Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8152Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8164Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers, e.g. poly (methyl vinyl ether-co-maleic anhydride)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/817Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Compositions or derivatives of such polymers, e.g. vinylimidazol, vinylcaprolactame, allylamines (Polyquaternium 6)
    • A61K8/8182Copolymers of vinyl-pyrrolidones. Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/12Preparations containing hair conditioners

Abstract

Disclosed herein are hair-mending compositions containing a polyelectrolyte complex. Also disclosed are methods of their use, methods of their manufacture, methods of testing their efficacy, and media methods involving hair mending.

Description

Hair maintenance compositions and correlation technique
The cross reference of related application
Present patent application requires the U.S. Provisional Patent Application 61/394,966 submitted on October 20th, 2010 and the priority of International Application Serial No. PCT/US 10/53360 of submitting on October 20th, 2010, and this both all incorporates this paper into by reference with it.
Background of invention
Hair care composition is usually through preparing to have multifrequency nature.For example, hair conditioner can through the preparation with conditioning hair, and can through the preparation with the maintenance hair.Hair care composition with multifrequency nature is attractive for consumers, because it only needs to use the effect that compositions still less just can obtain to expect to hair.Yet in order to prepare such hair care composition, various ingredients is normally essential.The long-time stability of such compositions may suffer damage due to the incompatibility between numerous components.
In addition, owing to having a large amount of components in many hair care compositions, formulator not only is faced with seeks suitable component with the challenge of cosmetic properties that expectation is provided, but also is faced with the challenge of making these complicated compositionss.Such challenge comprises that the Development and Production scheme makes compositions, no matter is for small-scale initial testing or for large-scale commercial market.The component of larger quantity mean need to larger quantity the manufacturing container, this itself namely means the more time of needs and consumes to produce described compositions.Cosmetic composition thereby be the complex mixture of various ingredients, and due to this complexity, just need careful consideration when the Development and Production scheme.
The component of hair care composition comprises conditioner, it typically is the compound with positive charge.Hair fiber has net negative charge.The positive charge of described conditioner is attracted to total negative charge of hair fiber, makes the conditioner with positive charge to described hair, affinity be arranged.This affine characteristic allows described conditioner and hair to interact, thereby makes conditioner that its opsonic action is provided.Described opsonic action restores hair fiber after can being included in the hair damage, for example repairs the end of bifurcated.
Conditioner known in the art comprises the quaternary nitrogen compound that is called " quaternary ammonium salt ", and the polymer that is called the group that comprises this compound of " polyquaternary ammonium salt ".Described polyquaternary ammonium salt comprises polyquaternary ammonium salt-28, vinyl pyrrolidone/methacryl amido oxypropyl trimethyl ammonium chloride copolymer.Have been found that polyquaternary ammonium salt-28 and methyl vinyl ether/maleic acid (PVMMA) with the combination results of specific ratios the compound polyelectrolyte (PEC) (U.S. Patent Application Publication No. 2005/0089494 and 2006/0251603 both all is transferred to ISP Investments Inc.) that damages of maintenance furcated end.Yet in the complex environment of hair nursing preparation, the stability of PEC may suffer damage due to the existence of other component, especially can destroy charging cpd and the polymer of PEC structure.Thus, the suitability of PEC just may be subject to them and the restriction of the compatibility of other component that expectation comprises in hair care composition.Because usually need multifrequency nature in hair care composition, so will expect to prepare the hair care composition of the stable combination of other hair nursing component that comprises PEC and other desired characteristic is provided.
And although PVMMA: polyquaternary ammonium salt-28PEC only forms component by two kinds and consists of, and the method for making these PEC is described to comprise two or three independent container in ISP Investment application.Such method is complicated, especially due to needs arbitrarily other container introduce other component.In full-scale plant with two or three container for the preparation of a kind of complex be inefficiency and be expensive.
Additionally, when consumer bought hair care product, consumer really was based on the characteristic of described hair care product and buys.For example, hair hair dry consumer may buy be used to making the barren dry product of hair, and the consumer of hair with furcated end may buy the product for the described furcated end of maintenance.Therefore, consumer may buy the hair care product that has for the desired characteristic of specific hair form or hair problem.For consumer's contrast hair care product compositions is bought about any decision to make, the advantageous feature of compositions clearly should be conveyed to consumer.A kind of method is to use photography, for example described in the ISP Investments application.Yet, need other method.
Therefore, needs are prepared stable hair care composition, it comprises unaffected PEC and other hair beneficial agent, especially charged hair beneficial agent.And, exist for for the preparation of PEC with comprise the demand of effective method more of the hair care composition of PEC.In addition, need the development and testing method with the result of improving of the furcated end maintenance that demonstrates hair care composition, make the benefit of hair care composition then can effectively be conveyed to consumer.Also need to develop the additive method that can show the hair care composition benefit, make described benefit then can effectively be conveyed to consumer.The invention provides these advantages.Other advantage of the present invention and other creative feature will be by highlighting in this paper description of this invention.
Summary of the invention
In one aspect, the invention provides the hair care composition of Emulsion form, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer, with respect to the comparative composition that contains multiple such compound polyelectrolyte, has the freeze-thaw stability of improvement.
In one aspect of the method, the invention provides hair care composition, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer, and the viscosity of wherein said compositions is greater than 3000 centipoises.
In one aspect of the method, the invention provides hair care composition, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer; Approximately 1% to about 5% thickening agent; Approximately 10% or more propylene glycol; And approximately 5% or more emollient; Wherein percentage ratio is based on the gross weight meter of described compositions.
In again aspect another, the invention provides hair care composition, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer; Approximately 3% to about 5% thickening agent; And approximately 2% or emollient still less; Wherein percentage ratio is based on the gross weight meter of described compositions.
The present invention also provides the method for using compositions as herein described, and it comprises the method for the furcated end of the method for conditioning hair fiber and maintenance hair fiber.
In addition, the invention provides the method for freeze-thaw stability of hair care composition that comprises the compound polyelectrolyte of cation type polymer and anionic polymer for improvement, described method comprises and will approximately 1% join in described hair care composition to about 5% thickening agent, and wherein the percentage meter is based on the gross weight meter of described compositions.
Additionally, the invention provides the method for freeze-thaw stability that comprises the hair care composition of compound polyelectrolyte for improvement, described method comprise with approximately 10% or more propylene glycol join in described hair care composition, wherein percentage ratio is based on the gross weight meter of described compositions.
The present invention also provides the method for the heat protection hair by using hair composition as described herein.
In addition, one aspect of the present invention provides the method for preparing compound polyelectrolyte, and described method is included in the methyl vinyl ether that will have in container as shown in the formula the repetitive of (formula I)/maleic acid hydration
Figure BPA00001701982700041
Make described methyl vinyl ether/maleic acid in described container with the alkali reaction of the amount that is enough at least part of its acidic-group of neutralization to form intermediate blend; Heat the described intermediate blend in described container; Add the vinyl pyrrolidone as shown in the formula (formula II) in described intermediate blend in the described container
With the methacryl amido oxypropyl trimethyl ammonium chloride as shown in the formula (formula III)
Cationic copolymer; And the described polymer in being blended in described container at high shear force with at least about the temperature of 50-60 ℃ prepares described compound polyelectrolyte.
The present invention also provides the method for preparing compound polyelectrolyte, and described method is included in the methyl vinyl ether of the repetitive that will have formula I in container/maleic acid hydration; Described methyl vinyl ether/maleic acid is reacted with for example 20% sodium hydroxide solution in described container, wherein said sodium hydroxide is for example to be enough to obtain approximately 6.5 to approximately 7.5 or approximately 6.9 adding to the about amount of 7.0 pH, to form intermediate blend; Described intermediate blend in described container is heated to approximately 50 ℃ to the about temperature of 60 ℃; The cationic copolymer of the methacryl amido oxypropyl trimethyl ammonium chloride of the vinyl pyrrolidone of formula II and formula III is added in described intermediate blend in described container; And mix described polymer in described container at high shear force and at least about the temperature of 50-60 ℃ at least about preparing described compound polyelectrolyte in 10 minutes.In one embodiment, described method also comprises described compound polyelectrolyte and one or more is selected from step that the composition of aqueous carrier, surfactant, flavouring agent, conditioner, emollient, emulsifying agent, thickening agent, antiseptic, gellant, siloxanes, hair-strengthening agent, wetting agent and wetting agent mixes to form hair care composition.In one embodiment, described mixing is enough to allow the abundant combination of described one or more compositions.
The method that the present invention also provides preparation to comprise the hair care composition of compound polyelectrolyte, it comprises the steps: will to have the methyl vinyl ether of the repetitive of formula I/maleic acid hydration in container; Make described methyl vinyl ether/maleic acid in described container be enough to the alkali of the amount of at least part of its acidic-group of neutralization, for example 20% sodium hydroxide solution reaction, for example wherein said sodium hydroxide is for example to be enough to obtain approximately 6.5 to approximately 7.5 or approximately 6.9 adding to the about amount of 7.0 pH, to form intermediate blend; With the heating of the described intermediate blend in described container for example to approximately 50 ℃ to the about temperature of 60 ℃; The cationic copolymer of the methacryl amido oxypropyl trimethyl ammonium chloride of the vinyl pyrrolidone of formula II and formula III is added in described intermediate blend in described container; The described polymer that mixes in described container at high shear force and at least about the temperature of 50-60 ℃ prepares described compound polyelectrolyte; One or more other compositions that are selected from aqueous carrier, surfactant, flavouring agent, conditioner, emollient, emulsifying agent, thickening agent, antiseptic, gellant, siloxanes, hair-strengthening agent, wetting agent and wetting agent are added in described compound polyelectrolyte in described container; And the compositions of mixing gained in container.In one embodiment, the hair care composition of described method preparation is the form of shampoo, conditioner, leave inorganic agent, cream, gel, mousse, essence, hair care oil, polishing material or spray.
The present invention also provides the method for preparing hair care composition, it comprises the compound polyelectrolyte of the cationic copolymer of preparation methyl vinyl ether/maleic acid and vinyl pyrrolidone and methacryl amido oxypropyl trimethyl ammonium chloride, and it comprises the steps: to make the methyl vinyl ether of the repetitive with general formula I/maleic acid hydration in the first container; Make described methyl vinyl ether/maleic acid in described the first container be enough to the alkali of the amount of at least part of its acidic-group of neutralization, for example 20% sodium hydroxide reaction, for example wherein said sodium hydroxide is for example to be enough to obtain approximately 6.5 to approximately 7.5 or approximately 6.9 adding to the about amount of 7.0 pH, to form intermediate blend; With the heating of the described intermediate blend in described the first container for example to approximately 50 ℃ to the about temperature of 60 ℃; The cationic copolymer of the methacryl amido oxypropyl trimethyl ammonium chloride of the vinyl pyrrolidone of formula II and formula III is added in described intermediate blend in described the first container; The described polymer that mixes in described the first container at high shear force and at least about the temperature of 50-60 ℃ prepares described compound polyelectrolyte; The component that one or more is selected from aqueous carrier, surfactant, flavouring agent, conditioner, emollient, emulsifying agent, thickening agent, antiseptic, gellant, siloxanes, hair-strengthening agent, wetting agent and wetting agent in second container is mixed; And described first or second container in the described compound polyelectrolyte of described the first container and the blending ingredients of described second container are mixed.In one embodiment, the hair care composition of described method preparation is the form of shampoo, conditioner, leave inorganic agent, cream, gel, mousse or spraying.
In addition, the invention provides the method for the reparation of the furcated end by the image reconstruction hair fiber, described method comprises hair fiber is fixed to the surface, and the described hair fiber that wherein is fixed to described surface has furcated end or be damaged to produce furcated end on described surface the time; Described surface is associated with multiplying arrangement, and wherein said furcated end is placed in the visual field of described multiplying arrangement; Image-capturing apparatus is associated, in order to catch the enlarged image of the visual field of described multiplying arrangement with described multiplying arrangement; With the described furcated end of compositions-treated, wherein said compositions, repairs described furcated end, and wherein said furcated end merges; And by the described image-capturing apparatus that is associated with described multiplying arrangement, catch the image of the reparation of described furcated end during described compositions-treated, and store the representative image of the reparation image that catches, be used for retrieval subsequently.In one embodiment, described compositions for example comprises approximately 1% to about 5% thickening agent, approximately 10% or more propylene glycol and approximately 5% or more emollient, and percentage ratio wherein is based on the gross weight meter of compositions.In another embodiment, described compositions comprises approximately 3% to about 5% thickening agent and approximately 2% or still less emollient, and percentage ratio wherein is based on the gross weight meter of compositions.In another embodiment, furcated end hair fiber reparation degree is communicated to consumer.
The present invention also provides qualitative assessment furcated end hair fiber to repair the method for degree, and described method comprises the acquisition wisp of hair, and wherein said hair is the hair of twice bleaching; Combing also dries up this bundle hair to make at least at least one furcated end in a hair fiber; Intrafascicularly remove the hair fiber that at least one has furcated end from this; The described at least one hair fiber of labelling randomly; Catch the first image of the furcated end of described at least one hair fiber, and store representative image, for example electronics representative image of described image; Described hair fiber is associated from the bundle that wherein removes with described hair fiber; With the described bundle of compositions-treated and described hair fiber; From the handled intrafascicular described hair fiber that removes; Seizure is from the second image of the handled intrafascicular described hair fiber end that removes; For described hair fiber, numerical value 0 is appointed as furcated end reparation, 1/2 is that part is repaired, perhaps 1 is reparation fully, with the reparation degree of the furcated end of assessing described hair fiber; And if many hair fibers are evaluated, randomly determine meansigma methods for the hair fiber of assessing.In one embodiment, described compositions for example comprises approximately 1% to about 5% thickening agent, and approximately 10% or more propylene glycol, and approximately 5% or more emollient, percentage ratio wherein is based on the gross weight meter of compositions.In another embodiment, described compositions comprises approximately 3% to about 5% thickening agent, and approximately 2% or emollient still less, percentage ratio wherein is based on the gross weight meter of compositions.In another embodiment, the degree of the hair fiber reparation of furcated end is communicated to consumer.
An embodiment of the invention provide qualitative assessment furcated end hair fiber to repair the method for degree, and described method comprises the acquisition wisp of hair; Make this at least one intrafascicular hair fiber to have furcated end; From the described intrafascicular at least one hair fiber with furcated end that remove; The described at least one hair fiber of labelling randomly; Catch the first image of the furcated end of described at least one hair fiber, and the representative image of storing described image, for example electronics representative image; Described hair fiber is associated from the bundle that wherein removes with described hair fiber; With the described bundle of compositions-treated and described hair fiber, wherein, described compositions comprises hair care composition, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer, approximately 1% to about 5% thickening agent, approximately 10% or more propylene glycol, and approximately 5% or more emollient, percentage ratio wherein is based on the gross weight meter of compositions; From the handled intrafascicular described hair fiber that removes; Seizure is from the second image of the handled intrafascicular hair fiber end that removes; For described hair fiber, numerical value 0 is appointed as furcated end reparation, 1/2 is that part is repaired, and perhaps 1 is reparation fully, with the reparation degree of the furcated end of assessing described hair fiber; And if many hair fibers are evaluated, randomly determine meansigma methods for the hair fiber of assessing so.
Another embodiment of the invention provides the method for the degree of qualitative assessment furcated end hair fiber reparation, and described method comprises the acquisition wisp of hair; Make at least one hair fiber of this bundle to have furcated end; Remove at least one hair fiber with furcated end from described bundle; The described at least one hair fiber of labelling randomly; Catch the first image of the furcated end of described at least one hair fiber, and representative image, for example electronics representative image of storing described image; Make described hair fiber be associated from the bundle that wherein removes with described hair fiber; Utilize the described bundle of compositions-treated and described hair fiber, wherein, described compositions comprises hair care composition, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer, approximately 3% to about 5% thickening agent, approximately 2% or emollient still less, percentage ratio wherein is based on the gross weight meter of compositions; From the handled intrafascicular described hair fiber that removes; Seizure is from the second image of the handled intrafascicular hair fiber end that removes; For described hair fiber, numerical value 0 is appointed as furcated end reparation, 1/2 is that part is repaired, and perhaps 1 is reparation fully, with the reparation degree of the furcated end of assessing described hair fiber; And if many hair fibers are evaluated, so randomly determine the meansigma methods of the hair fiber assess.
Another embodiment of the invention provides the method for the degree that the hair fiber of qualitative assessment end bifurcated repairs, and described method comprises the acquisition wisp of hair; Make at least one hair fiber of this bundle to have furcated end; Remove at least one hair fiber with furcated end from described bundle; The described at least one hair fiber of labelling randomly; Catch the first image of the furcated end of at least one hair fiber, and representative image, for example electronics representative image of storing described image; Described hair fiber is associated from the bundle that wherein removes with described hair fiber; With the described bundle of compositions-treated and described hair fiber, wherein, described compositions comprises hair care composition, and it comprises the compound polyelectrolyte of cation type polymer and anionic polymer, and wherein, the viscosity of described compositions is greater than 3000 centipoises; From the handled intrafascicular described hair fiber that removes; Seizure is from the second image of the handled intrafascicular hair fiber end that removes; For described hair fiber, numerical value 0 is appointed as furcated end reparation, 1/2 is that part is repaired, and perhaps 1 is reparation fully, with the reparation degree of the furcated end of assessing described hair fiber; And if many hair fibers are evaluated, so randomly determine the meansigma methods of the hair fiber assess.
Another embodiment of the invention provides the method for reparation degree of the hair fiber of qualitative assessment end bifurcated, and described method comprises the acquisition wisp of hair; Make this at least one intrafascicular hair fiber to have furcated end; Remove at least one hair fiber with furcated end from described bundle; The described at least one hair fiber of labelling randomly; Catch the first image of the furcated end of described at least one hair fiber, and store representative image, for example electronics representative image of described image; Described hair fiber is associated from the bundle that wherein removes with described hair fiber; With the described bundle of compositions-treated and described hair fiber, wherein, described compositions comprises the hair care composition of Emulsion form, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer, and this hair care composition has the freeze-thaw stability of improvement with respect to the comparative composition that contains multiple such compound polyelectrolyte; From the handled intrafascicular described hair fiber that removes; Seizure is from the second image of the handled intrafascicular hair fiber end that removes; For described hair fiber, numerical value 0 is appointed as furcated end reparation, 1/2 is that part is repaired, and perhaps 1 is reparation fully, with the reparation degree of the furcated end of assessing described hair fiber; And if many fibers are evaluated, so randomly the meansigma methods of definite hair fiber of assessing.
Description of drawings
Fig. 1 is block diagram, has shown to use method of the present invention to utilize the determined reparation percentage ratio of washing-off type conditioner in three circulations.Numerical value in round parentheses is compound polyelectrolyte (PEC) percentage ratio.The fiber number of testing for different components is 20,100 and/or 50.
Fig. 2 is block diagram, shows to use method of the present invention to utilize the determined reparation percentage ratio of leave compositions in a processing.20 fibers have been tested for every kind of compositions.
Fig. 3 uses compound polyelectrolyte (PEC) to repair the figure of furcated end for showing.Described figure has shown the mechanism of being repaired furcated end by PEC: PEC is attached to the position of furcated end, and self forms network, and the fiber assembling is also shunk along with their drying, and furcated end thus internally bonds.
Fig. 4 A-4D has also shown the image of the reparation of various furcated end types.
Fig. 5 has also shown the still image of the restored video that picks up from furcated end in repair process.
Fig. 6 is the schematic diagram according to the image data collection system of embodiment of the present invention.
Fig. 7 has shown the relatively line diagram of the high humility crimp retention of exemplary composition of the present invention.
Fig. 8 has shown the heat protection of the hair that uses exemplary composition of the present invention.
What Fig. 9-19 had shown compositions described herein freezes/melts comparison.
Figure 20 has shown the furcated end of repairing by exemplary composition of the present invention.
Detailed Description Of The Invention
The present invention is based on the astonishing and unexpected discovery of the stable composition that comprises compound polyelectrolyte (PEC) and other hair beneficial agent (particularly charge species), wherein, described PEC keeps complete and shows hair repairing effect.Unexpected discovery PEC can with other charged hair beneficial agent---namely have the material of beneficial characteristics or give the material of beneficial characteristics to hair for hair, cationic conditioner for example---combine, and can not destroy the complex of definition PEC structure.Due to this unexpected discovery, compositions provided by the invention not only provides the hair repairing effect of PEC, but also the advantage of other hair beneficial agent is provided.Thus, the invention provides compositions and the method that comprises such as charged hair beneficial agent---such as quaternary ammonium salt, cationic conditioning polymer etc.---.The suitable hair beneficial agent that can combine with PEC according to the present invention comprises, for example SAPDMA, cocamido propyl betaine, polyquaternary ammonium salt-37, polyquaternary ammonium salt-7, polyquaternary ammonium salt-39, DC 5-7113 (polysiloxane quaternary ammonium-16 and tip-nip polyethers-11 and butyl capryl alcohol and tip-nip polyethers-5),
Figure BPA00001701982700101
T Quat 60 (polysiloxane quaternary ammonium-22), quaternary ammonium salt-80,
Figure BPA00001701982700102
2001 (polyquaternary ammonium salt-47) and acrylic acid/VP cross linked polymer.This paper describes the charged hair beneficial agent that other is suitable.
The present invention also provides the single vessel process for the preparation of PEC.Method of the present invention also allows to prepare the identical PEC of the prepared PEC of particle size distribution and the conventional method that needs to adopt two or more independent containers.Thus, the invention provides for the preparation of PEC and comprise the more effectively and cheaply method of the hair care composition of PEC.
The present invention also allows the concentration of PEC greater than 4 % by weight, for example 8 % by weight.
Additionally, the present invention have advantages of provide can picture specification hair care composition benefit method, make described benefit then can effectively convey to consumer.Consumer is based on the characteristic of hair care product and buy hair care product.Like this, it is very important that the beneficial characteristics of hair care product compositions is conveyed to these consumers effectively, makes consumer can make astute purchase decision when the hair care product of comparative competition.
The present invention also further has advantages of the method for testing of improving result that the furcated end reparation that allows to demonstrate hair care composition is provided, and makes the benefit of hair care composition then can effectively be conveyed to consumer.Most furcated end recovery test method uses end by the original hair of mechanical induction bifurcated.Use original hair can make the composition of furcated end remediation composition capable only act on the damage of mechanical induction.In other words, in original hair, there is not other damage except described furcated end.Therefore, remediation composition capable can be guided its repair ability and only be acted on the furcated end damage.Like this, the reparation composition of compositions will can not wasted on the other parts of hair.Yet found to have other damage the hair of (for example due to bleaching) can be used to substitute original hair in furcated end recovery test method unexpectedly.This is counterintuitive because desired be that any remediation composition capable will make it repair component being adsorbed to other damage of hair, and be not only furcated end, thereby reduce the amount of repairing furcated end.It is more serious that the applicant has been found that hair damages, and the reparation of furcated end is better.And, have been found that and use badly damaged hair more, can obtain the high percentage ratio of repairing in rinse-off products, for example higher than 50%, it is obtainable level in the leave product.In one aspect, the invention provides the hair care composition of Emulsion form, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer, and this hair care composition has the freeze-thaw stability of improvement with respect to comparative composition (for example the PEC described in U.S. Patent Application Publication 2005/0089494 and 2006/0251603 is formulated in conventional hair nursing base formulation and makes).In embodiment, described compositions comprises, for example approximately 1% to about 5% thickening agent, and approximately 10% or more propylene glycol, and approximately 5% or more emollient, percentage ratio wherein is based on the gross weight meter of compositions.In another embodiment, described compositions comprises approximately 3% to about 5% thickening agent, and approximately 2% or emollient still less, percentage ratio wherein is based on the gross weight meter of compositions.
Compositions of the present invention provides unforeseeable freeze-thaw stability.Freeze-thaw stability is the key property of hair care composition, particularly for often compositions being exposed to the purpose of transportation and the storage of low temperature extreme condition.Freeze-thaw stability is also important for being retained in the product that also is exposed to thus the open air of extreme temperature on hair.The compositions that contains PEC is not unsettled inherently freezing/melt under condition.Yet, when with use in the art with the thickening agent compositions one or more aliphatic alcohol (cetyl, stearyl aliphatic alcohol etc.) with for example approximately 3 % by weight or higher (for example approximately 5 % by weight) in conjunction with the time, preparation will be unsettled during freezing/melting.Described compositions will become granular and tubbiness, and this is not satisfied for consumers, and might be repelled by consumer.
Except freezing/melt unstability, the conventional composition with 5% aliphatic alcohol of having an appointment containing of PEC does not have long term high temperature stability.The viscosity of such compositions continue to increase along with the time (for example after 45 ℃ of lower 2-3 months over 100,000 centipoise), this is not satisfied for consumers, can not be dispersed on whole hair because it is too thick and hard, and may be repelled by consumer.The inventor has been found that
Figure BPA00001701982700121
The membership that adds improve viscosity and control; That is, control viscosity and for example remain on approximately 20,000-40,000 centipoise.
The compositions and methods of the invention can comprise thickening agent.Thickening agent increases the viscosity of compositions, makes the compositions with more substantial given thickening agent have higher viscosity.Described thickening agent can be for example quaternary nitrogen compound or polymer, polyquaternary ammonium salt-37 for example, and polyquaternary ammonium salt-37th wherein for example are with the mixture of propylene glycol dicaprylate/dicaprate and polypropylene glycol-1 tridecyl alcohol polyethers-6 (polypropylene glycol-1 trideceth-6).From
Figure BPA00001701982700122
/ BASF, Basel, Switzerland's
Figure BPA00001701982700123
SC 96 is examples of such mixture.
Figure BPA00001701982700124
SC 96 is 65% polyquaternary ammonium salt-37,25% propylene glycol dicaprylate/dicaprate, 10%PPG-1 tridecyl alcohol polyethers-6.Other suitable thickening agent also can be added into compositions of the present invention, for example comprises xanthan gum, acrylic acid/VP cross linked polymer (Ultrathix for example TMP-100; ISP, Wayne, NJ, USA), PVP, PVP K-90, PEG-90M and styrene/VP copolymer.
In one aspect of the method, the invention provides hair care composition, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer, and the viscosity of wherein said compositions is greater than 3000 centipoises.In embodiment, such compositions for example can comprise approximately 1% to about 5% thickening agent, approximately 10% or more propylene glycol, and approximately 5% or more emollient, wherein percentage ratio is based on the gross weight meter of compositions.In another embodiment, such compositions for example can comprise approximately 3% to about 5% thickening agent, and approximately 2% or emollient still less, wherein percentage ratio is based on the gross weight meter of compositions.
The viscosity of the present composition is based on the amount of the thickening agent that adds and/or other component and change.Compositions of the present invention can comprise concentration be approximately 1 % by weight to the about thickening agent of 10 % by weight.The % by weight amount of described thickening agent can be for for example listed in following table.In described table, " X " expression scope " from [respective value the first row] to [respective value in first row] ".For example, first " X " is the scope of " from about 1 % by weight to about 2 % by weight ".
Table 1
Figure BPA00001701982700131
Thus, viscosity can have the scope between any above-mentioned end points.
The range of viscosities of the present composition can for for example approximately 3000 centipoises to approximately 100,000 centipoise, perhaps for example approximately 20,000 centipoise is to about 40,000 centipoises, for less than 50, the viscosity of 000 centipoise obtained 25 ℃ of tests with 10rpm by RV T-B in 1 minute, or for the viscosity less than 100,000 centipoises obtained 25 ℃ of tests with 5rpm by RV T-C in 1 minute greater than 50,000 centipoises.The range of viscosities of the present composition can be for for example listed in following table.In described table, " X " expression scope " from [respective value the first row] to [respective value in first row] ".For example, first " X " is the scope of " from about 3000 centipoises to about 10,000 centipoises ".
Table 2
Thus, described viscosity can have any two scopes that define by above-mentioned end points.
In one aspect of the invention, compositions comprises thickening agent, and the emollient of propylene glycol and relative high concentration is for example with 5 % by weight or higher amount.Suitable emollient can comprise for example one or more aliphatic alcohol.The hair care product that consumer may find to contain 10 % by weight or more propylene glycol is unacceptable, they may think that such product has thick and heavy and sticky sensation, may notice that hair can spend the long time dry (due to the wetting characteristics of glycol), may notice that perhaps hair is difficult to combing or lackluster.Yet, surprisingly, have now found that according to the present invention includes 10% or more propylene glycol acceptable freeze-thaw stability not only is provided, and can provide more the compositions that may accept for consumer.Additionally, the applicant has been found that the Emulsion of this compositions can accept high-caliber glycol and can not be affected (such as viscosity variation etc.).The applicant finds other polyhydric alcohol, for example Sorbitol and the glycerol of 5 % by weight can't provide acceptable freeze-thaw stability.
In some embodiments, the compositions and methods of the invention can comprise propylene glycol, for example with about 10 % by weight or larger, and about 20 % by weight or larger, about 30 % by weight or larger, about 40 % by weight or larger, perhaps approximately 50 % by weight or larger concentration.
The present invention also provides hair care composition, and it comprises the compound polyelectrolyte of cation type polymer and anionic polymer; Approximately 1% to about 5% thickening agent; Approximately 10% or more propylene glycol; With approximately 5% or more emollient; Wherein percentage ratio is based on the gross weight meter of compositions.
In another aspect, the invention provides hair care composition, it comprises the compound polyelectrolyte of cation type polymer and anionic polymer, and approximately 3% to about 5% thickening agent, with approximately 2% or still less emollient, wherein percentage ratio is based on the gross weight meter of compositions.In this one side, compositions of the present invention preferably is substantially free of propylene glycol.As used herein, " being substantially free of propylene glycol " and meaning compositions of the present invention contains and is less than the approximately propylene glycol of 1 % by weight, be less than the approximately propylene glycol of 0.5 % by weight, be less than the approximately propylene glycol of 0.1 % by weight, and 0 % by weight or do not contain propylene glycol more preferably.
Can there be one or more emollient in the compositions and methods of the invention.Emollient can for example soften and/or the skin of releiving.Suitable emollient can comprise for example aliphatic alcohol.Aliphatic alcohol comprises for example spermol, stearyl alcohol and combination thereof.Sometimes use aliphatic alcohol with thickener composition and the skin moistening characteristic is provided.The applicant it has surprisingly been found that compositions of the present invention, for example 5% aliphatic alcohol/1%
Figure BPA00001701982700151
SC 96 and 1% aliphatic alcohol/5% SC 96, roughly show identical Emulsion characteristic (for example viscosity, rheological characteristic, yield value, outward appearance, color).This is unexpected in the spermol lowering of concentration to only for about 1 % by weight the time.In addition, now have been found that in the compositions of the PEG with 2 % by weight, in the situation that compositions also has approximately 3 % by weight to the about thickening agent of 5 % by weight, emollient concentration can be reduced to approximately 1 % by weight or lower.The % by weight scope of aliphatic alcohol can increase when the concentration of PEC is lower.Or even when the skin moistening aliphatic alcohol of low concentration, find that the PEC compositions still provides acceptable sense learning through practice.This thinks that at most skin moistening aliphatic alcohol with higher concentration consumer provides the hair care composition of sense learning through practice, is especially unexpected in conditioner.And, combining with thickening agent, the PEC compositions has kept acceptable viscosity.Additionally, the skin moistening aliphatic alcohol of low concentration and have the sufficient White-opalescent that about 3 % by weight to the about combination of the PEC of 5 % by weight thickening agents provides these components arbitrarily can't observe separately.
In the present composition concentration of emollient can be desirably based on the concentration of thickening agent and regulate.For example for the thickening agent of 3-5 % by weight, the emollient concentration range can be for for example listed in following table.In described table, " X " expression scope " from [respective value of the first row] to [respective value of first row] ".For example, first " X " is the scope of " from about 0 % by weight to about 0.1 % by weight ".
Figure BPA00001701982700171
Figure BPA00001701982700181
Therefore, the concentration of emollient can have any two scopes that define by aforementioned end points.Replacedly, for example for the thickening agent of 1-5 % by weight, emollient concentration can be for example approximately 5 % by weight or larger, approximately 6 % by weight or larger, about 7 % by weight or larger, approximately 8 % by weight or larger, approximately 9 % by weight or larger, approximately 10 % by weight or larger, about 20 % by weight or larger, about 30 % by weight or larger, about 40 % by weight or larger, perhaps about 50 % by weight or larger.
Some PEC describes in U.S. Patent Application Publication 2005/0089494 and 2006/0251603, and the two all incorporates this paper into by reference with it.As summarizing in these are open, the formation of PEC is not simply due to the polymer that has oppositely charged in compositions.Existing polymer-polymer material in the time of can making phasor with the concentration change of the polymer that is presented at oppositely charged (changing thus the ratio of polymer between mutually).Based on described phasor, can determine the ratio of polymer aspects such as percentage by weight, molal quantity when forming PEC.For PVMMA/ polyquaternary ammonium salt-28PEC, preferred weight rate is the PVMMA of 1: 9: polyquaternary ammonium salt-28.Yet PEC can exist under other percentage by weight ratio.For example, PVMMA/ polyquaternary ammonium salt-28PEC can form at about 1: 9 percentage by weight ratio, makes slightly higher than or will have a certain amount of PEC lower than the ratio of 1: 9 to exist.The percentage by weight ratio ranges can be approximately 1: 8 to the about PVMMA of 1: 10: polyquaternary ammonium salt-28.Thus, in the present composition and the weight rate of the active matter of the cation type polymer that uses in the methods of the invention and anionic polymer be approximately 1: 8 to approximately 1: 10.
Except the percentage by weight ratio, the formation of PEC can be based on the electric charge of polymer-electric charge ratio and is determined.PEC is to form in 1: 1 o'clock at the electric charge of polymer-electric charge ratio usually.Therefore, PEC may form during by the positive charge of another polymer institute balance at each negative charge of polymer.Yet PEC can exist under other electric charge-electric charge ratio.For example, PEC can form at about 1: 1 electric charge-electric charge ratio, make slightly higher than or will have a certain amount of at least PEC lower than the ratio of 1: 1 to exist, for example, as the ratio of 0.82 to 1.8 cation ratio anionic charge under.Can make phasor and have situation to determine PEC under different electric charges-electric charge ratio.
PEC of the present invention can be by the polymer that comprises cationic charge and the polymer formation that comprises anionic charge.Yet, as long as polymer interacts by ionic bond, can form the suitability of PEC with definite polymer arbitrarily-polymeric system by tectofacies map.The compositions and methods of the invention can comprise compound polyelectrolyte, wherein, cation type polymer comprises the one or more monomeric units with one or more quaternary nitrogen groups, for example vinyl pyrrolidone/methacryl amido oxypropyl trimethyl ammonium chloride copolymer (polyquaternary ammonium salt-28).The limiting examples that can be used to form other cation type polymer of PEC comprises other polyquaternary ammonium salt polymer, for example polyquaternary ammonium salt-7, Polyquaternium-10 or polyquaternary ammonium salt-11.The compositions and methods of the invention can comprise compound polyelectrolyte, and wherein, anionic polymer comprises the monomeric unit with ionizable hydroxy-acid group, for example methyl vinyl ether/maleic acid.Another example that can be used to form the anionic polymer of PEC is vinyl pyrrolidone/acrylate/lauryl methacrylate copolymer.
Polymer with ionogen, for example hydroxy-acid group or tertiary amine group may need to regulate pH, to form compound polyelectrolyte.The adjusting of pH has changed the percentage ratio of ionizable ionogen, and has therefore regulated and can pass through ionic bond and interactional group quantity.Can use the suitable pH of phasor to determine that PEC forms for preparing under different pH.For PVMMA/ polyquaternary ammonium salt-28PEC, approximately 6.5 can be used to form PEC to about 7.5 pH scope.Suitable pH scope can be for example as listed in following table.In described table, " X " expression scope " from [respective value the first row] to [respective value in first row] ".For example, first " X " is scope " from about pH6.5 to about pH6.6 ".
Table 4
Figure BPA00001701982700201
Therefore, pH can have any two scopes that define by aforementioned end points.
The pH of compositions can regulate with nertralizer/buffer agent.For acidic-group carboxylic acid for example, can use antalkali, for example hydroxide compound.Suitable hydroxide compound comprises highly basic, for example sodium hydroxide.For basic group, can use acid acceptor, for example citric acid.Can use any suitable nertralizer concentration, for example comprise which listed those in following table.In described table, " X " expression scope " from [respective value of the first row] to [respective value of first row] ".For example, first " X " is scope " from about 0.1 % by weight to about 1 % by weight ".
Table 5
Therefore, the concentration of nertralizer can have any two scopes that define by aforementioned end points.As long as described PEC forms under the pH condition of expectation, comprise that the final pH of compositions of any gained of PEC can be identical or different from the pH that PEC forms, complete as long as PEC keeps.
Described PVMMA/ polyquaternary ammonium salt-28PEC has the ability of the furcated end of repairing hair fiber.Hair has net negative charge.Do not limited by any specific theory, PEC is considered to hair fiber affine (substantive), and is bonded together by the end of adhesive property with furcated end.The positive charge of polyquaternary ammonium salt-28 polymer attracted to electronegative hair fiber, and is affine to hair.Because electronegative PVMMA polymer by compound to polyquaternary ammonium salt-28, so PVMMA also attracted on hair.Then end and/or its each other the interaction of the end of furcated end by a plurality of PEC and furcated end produces cementation, thereby is attached to together (for example in the situation that the film that film shrinks during drying form in).Additionally, the surface tension that is experienced due to the interaction of water in the film forming process by the end of furcated end helps end is bonded together.
As long as PEC is suspending or the form of emulsified particles exists, the particle size of PEC just should allow PEC to enter into the end of furcated end, so that the impaired hair fiber of PEC reparation.As long as PEC can enter the end of furcated end, particle size distribution can have any suitable mean P EC particle size.Suitable mean P EC particle size for example can comprise as listed those in following table.In described table, " X " expression scope " from [respective value the first row] to [respective value in first row] ".For example, first " X " is the scope of " from about 0.5 μ m to about 1 μ m ".
Table 6
About 0.5 μ m About 1 μ m About 2 μ m About 3 μ m About 5 μ m About 10 μ m About 20 μ m About 30 μ m
About 1 μ m X
About 2 μ m X X
About 3 μ m X X X
About 5 μ m X X X X
About 10 μ m X X X X X
About 20 μ m X X X X X X
About 30 μ m X X X X X X X
About 40 μ m X X X X X X X X
Therefore, mean P EC particle size distribution can have any two scopes that define by aforementioned end points.In some embodiments, the PEC distribution of particles that comprises of the compositions and methods of the invention is: mean P EC particle size is approximately 5 microns, for example approximately 5 ± 3 microns or approximately 5 ± 2 microns.The compositions and methods of the invention can also comprise the PEC granule that is present in microgel, the microgel structure of for example interlocking.
The compositions and methods of the invention can contain higher than the PEC that is considered in the art before under accessible concentration.For example, compositions of the present invention can comprise the PEC with the PVMMA/ polyquaternary ammonium salt-28 of 8 % by weight concentration.The concentration of PEC can be different in hair care composition.The compositions and methods of the invention can contain in based on the gross weight of compositions approximately 1% to the about compound polyelectrolyte of 8% concentration.Compositions of the present invention can contain in based on the gross weight of compositions approximately 1% to approximately 3% or approximately 2% to the about compound polyelectrolyte of 4% concentration.The concentration of PEC can be for example as listed in following table.In described table, " X " expression scope " from [respective value the first row] to [respective value in first row] ".For example, first " X " is scope " from approximately 0.1% to approximately 0.5% ".
Table 7
Approximately 0.1% Approximately 0.5% Approximately 1% Approximately 2% Approximately 3% Approximately 4% Approximately 5% Approximately 6% Approximately 7%
Approximately 0.5% X
Approximately 1% X X
Approximately 2% X X X
Approximately 3% X X X X
Approximately 4% X X X X X
Approximately 5% X X X X X X
Approximately 6% X X X X X X X
Approximately 7% X X X X X X X X
Approximately 8% X X X X X X X X X
Therefore, the concentration of PEC can have any two scopes that define by aforementioned end points.
The formation of PEC can be confirmed with any suitable method.The example of appropriate method comprises microscopy.Under optical microscope, structure that can Study Polymer Melts-polymeric system, and can determine with the size measuring software size of existing any granule.Such method can draw the particle size distribution of PEC, and prerequisite is that the existence of other component can not make the PEC structural fuzzy.Another kind method comprises with the Malvern Particle Size Analyzer determines particle size distribution.And, the only physical characteristic of the compositions of the PEC existence that can indicate PEC in carrier solvent.For example, along with the increase that PEC exists, the turbidity of this compositions and opacity increase.And for given polymer-polymeric system, the reduced viscosity of this compositions minima extremely is corresponding to the PEC that has maximum, and wherein said PEC is the finest and close.
Compositions of the present invention is following form, and the compositions of the method for the present invention following form that can make or use: such as shampoo, conditioner, gel, purificant, Emulsion (oil-in-water, Water-In-Oil or heterogeneous), emulsion, cream, unguentum, ointment, brilliantine, spray (pressurization or non-pressurised), injection, mousse, foam, shampoo, solution and solid (such as dope, semisolid etc.).Therefore, compositions of the present invention is following form, and the compositions of following form can be made or use to method of the present invention: the form of cream, emulsion, solution, ointment or gel for example.Therefore, hair care composition of the present invention and method can comprise other component of the compositions that can be suitable for these types.Preferably, such component and PEC are compatible, because described component can not destroyed the PEC structure.
Compositions is applicable to washing-off type, leave and/or the processing of spending the night.Method of the present invention and hair care composition can comprise that the composition that compound polyelectrolyte and one or more are selected from aqueous carrier, surfactant, nertralizer, flavouring agent, conditioner, emulsifying agent, thickening agent, antiseptic, gellant, siloxanes, hair-strengthening agent, wetting agent and wetting agent mixes to form hair care composition.Therefore, the compositions and methods of the invention can comprise for example antiseptic, nertralizer, flavouring agent, siloxanes or its combination.Those skilled in the art will recognize that the determined component of this paper can have multifrequency nature, and can adapt to the various ingredients classification thus, if especially it is for having multicomponent commercially available product.
Aqueous carrier can comprise the water of any appropriate amount, for example approximately 25 % by weight to the about water of 97 % by weight (for example approximately 30 % by weight to the about water of 95 % by weight).Compositions of the present invention can comprise approximately 30 % by weight to the about water of 97 % by weight, and approximately 50 % by weight are to the about water of 80 % by weight, perhaps approximately 60 % by weight to the about water of 70 % by weight.The water that uses in the present composition can be deionized water.
Suitable emulsifying agent for example can comprise PPG-3 benzylic ether myristinate (Crodamol STS for example; Croda, Inc., Edison, NJ, USA), arachidic alcohol and behenyl alcohol and Semen arachidis hypogaeae base glucoside (Montanov for example 202; SEPPIC, Paris, France), (for example SepigelTM 305 for polyacrylamide and C13-14 isoparaffin and laureth-7; SEPPIC), tristerin, different spermol polyethers-20, oleth-2, methoxyl group PEG/PPG-7/3 aminopropyl polydimethylsiloxane, PEG/PPG-18/18 polydimethylsiloxane (DC-190 for example; Dow Corning), PEG-12 polydimethylsiloxane, Cremophor RH40, PEG-6 caprylic/capric triglyceride, aminomethyl propanol (AMP-95) and polyglycereol-3 distearate.
Can use suitable surfactant, for example cleaning and/or detergent surfactant, comprise for example laureth disodium sulfosuccinate, sodium laureth sulfate, polysorbate20, polysorbate60, cocamido propyl betaine and stearyl dimethyl benzyl ammonium chloride (Stearalkonium chloride).Such surfactant may reside in shampoo composite.Conditioner preferably is substantially devoid of cleansing surfactants, unless described conditioner is the two-in-one combination of shampoo and conditioner.As used herein, " being substantially devoid of cleansing surfactants " refer to that compositions of the present invention contains and be less than the approximately cleansing surfactants of 2 % by weight, and more preferably less than about 1 % by weight, 0 % by weight or do not contain cleansing surfactants for example.
Suitable conditioner can comprise for example tertiary amine or quaternary amine, for example SAPDMA, polyquaternary ammonium salt-47 (Merquat for example 2001; Nalco, Naperville, IL, USA), siloxane quaternary ammonium-22 (for example
Figure BPA00001701982700252
T Quat 60; Evonik, Essen, Germany), cocamido propyl betaine, polyquaternary ammonium salt-11, polyquaternary ammonium salt-39, polyquaternary ammonium salt-4 (
Figure BPA00001701982700253
H-100; Akzo Nobel, Amsterdam, Netherlands), polyquaternary ammonium salt-4 (
Figure BPA00001701982700254
L-200; Akzo Nobel) to 0.5 % by weight, polyquaternary ammonium salt-7, Polyquaternium-10 and quaternary ammonium salt-80.Other suitable conditioner comprises for example Aqu D 4272N-Hance SP100 (acrylamide propyl trimethyl ammonium chloride/acrylamide copolymer), distearyl acyl group ethyl alkyl dimethyl ammonium chloride; Cetearyl alcohol (Varisoft EQ 65), Rhodia Guar S, mountain Yu base trimethyl ammonium chloride and mountain Yu base trimethyl ammonium chloride (Behentimonium Chloride)/cetearyl alcohol.Have been found that N-Hance SP100 copolymer is especially favourable.Therefore, the compositions and methods of the invention can comprise for example acrylamide propyl trimethyl ammonium chloride/acrylamide copolymer.As shown in the following Example 16, in containing the compositions of PEC, this copolymer provides extra furcated end repair.
Although optional, at least a antiseptic of effective dose can be incorporated in described compositions.For example, can select antiseptic to kill the antibacterial that may survive or breed in compositions in other situation.Suitable antiseptic can comprise for example DMDM Hydantoin, EDETATE SODIUM, Kathon TMCG (active component: CMIT and MIT) etc., and combination.
Can use suitable gellant.Suitable gellant for example can comprise acrylic acid/VP cross-linked copolymer (Ultrathix for example TMP-100; ISP).
Can add suitable siloxanes for example to improve the conditioning of hair.Suitable siloxanes can comprise for example polysiloxane-based, comprises polydimethylsiloxane, dimethiconol, cyclopentasiloxane and cyclohexasiloxane.These comprise for example poly-trimethicone of phenyl,
Figure BPA00001701982700261
OSW 5 (84% cyclopentasiloxane, 15% dimethiconol, 1% polydimethylsiloxane; Evonik, Essen, Germany), DC-200 (polydimethylsiloxane; Dow Corning, Midland, MI, USA), Fluid Blend (80% Cyclomethicone, 20% polydimethylsiloxane), and DC-1501 (D5/ polydimethylsiloxane; Dow Corning).Other suitable siloxanes for example comprises that (phenyl gathers trimethicone to DC-556; Dow Corning), siloxanes with amino-functional, DC-949 (31% ammonia end polydimethylsiloxane for example, 1.9% tridecyl alcohol polyethers-12,2.2% hexadecyltrimethylammonium chloride, 55-60% water, 2.2% ring four polydimethylsiloxane, 1.6% cyclopentasiloxane, and<0.5% sodium benzoate; Dow Corning), DC-8500 (82% pair of (C13-15 alkoxyl) PG-ammonia end polydimethylsiloxane, 18%C14-15 alcohol; Dow Corning), aminopropyl dimethione, DC 5-7113 siloxane quaternary ammonium microemulsion (66% water, 25% siloxane quaternary ammonium-16,7.4% tip-nip polyethers-11,4.5% butyl capryl alcohol, 3.5% tip-nip polyethers-5; Dow Corning), DC 2-8566 (ammonia end polydimethylsiloxane; Dow Corning), and ammonia end polydimethylsiloxane (ADM 1100; Wacker).
Can use suitable hair-strengthening agent.Suitable example comprises that for example VP/ methacrylic acid amino/the vinyl imidazole copolymer (for example
Figure BPA00001701982700262
Clear; BASF), acrylic acid/vinyl pyrrolidone cross linked polymer (UltrathixTM P-100 for example; ISP), caprolactam/VP/ dimethylaminoethyl methacrylate copolymer (
Figure BPA00001701982700263
S; And the VP/VA copolymer ISP).
Other component be can add, for example Cocoa Cortex cocois radicis (Cortex cocois radicis) oil, mineral oil (liquid paraffin), sodium chloride, hydrolyzed silkworm silk albumen, keratin aminoacid, ascorbic acid, panthenol, tocopheryl acetate, biotin, nicotiamide, triethanolamine, Fructus Tritici aestivi (Semen Tritici aestivi) flour lipid, ceramide 3, American Avocado Tree oil, tetrahexyldecyl ascorbate, Generol 122, alpha-glucans oligosaccharide, ethylhexyl methoxy cinnamate, butyl methoxydibenzoylmethise and tocopheryl acetate comprised.Propellant be can use, for example in spray composite, iso-butane and propane and 152A (78.5%A46 comprised; 28.5%HFC 152A).Can use fatty acid, for example myristic acid, Palmic acid and stearic acid.
Can provide other component and/or composition to think that hair gives favourable characteristic, for example be used for giving softness, moisture being provided, the homogeneity/viscosity of compositions pleasant and component and/or the composition that volume/plumpness is provided for hair are provided to hair for hair after drying.
Can provide flavouring agent in compositions of the present invention.The limiting examples of flavouring agent is the flower extract.Can use any concrete flavouring agent, and those skilled in the art will recognize that consistent especially flavouring agent is not important.In fact, can provide the compositions of the present invention that there is no flavouring agent.
The embodiment of the present composition can comprise 1-2 % by weight for example with the PVMMA copolymer of the ratio of 1: 9 and the PEC of polyquaternary ammonium salt-28.Such complex can prepare in the side line container and be added in main proportion container after breast is produced mutually with when described breast is cooled to 45-65 ℃ mutually.Approximately the tertiary amine of 1-2 % by weight or quaternary amine can be included in breast mutually in and be neutralized to the approximately pH of 4.0-6.0.Can comprise with the ratio of 5: 1 approximately the aliphatic alcohol of 3-7 % by weight (for example spermol and/or stearyl alcohol) and low HLB co-emulsifier, such as glyceryl monostearate, distearate etc., and can be included in breast mutually in.The mixture that can comprise the siloxanes of the siloxanes of 0.1-10 % by weight for example or polydimethylsiloxane, Cyclomethicone, phenyl and/or amino-functional.Can add the emollient ester with for example 1-4 % by weight, for example PPG-3 benzyl oxide myristinate (for example Crodamol STS) is to strengthen product spread and to strengthen glossiness and hair sense of touch.Can comprise that 10% propylene glycol freezes/melt stability with improvement.Can also comprise
Figure BPA00001701982700271
SC-96, it can and add to improve viscosity with for example 0.1-5 % by weight after the breast phase when batch of material is cooled to 45-65 ℃, improve the conditioning sensation in hair, and improves long-time stability and viscosity control.The another kind of embodiment of the present composition can comprise for example identical composition, except having approximately 1% aliphatic alcohol, does not contain the emollient ester, and SC-96 is for example 1-7 % by weight.Have approximately that the embodiment of the compositions of 3-7 % by weight aliphatic alcohol can comprise the PEC complex, it prepares in primary tank at first, and the remaining compositions of preparation in same containers then, wherein
Figure BPA00001701982700273
SC-96 has increased to for example 1-7 % by weight.Have approximately that the embodiment of the compositions of 1 % by weight aliphatic alcohol can comprise the PEC complex, it prepares in primary tank at first, and the remaining compositions of preparation in same containers then, wherein
Figure BPA00001701982700274
SC-96 increases to for example 3-10 % by weight.
The present invention includes by the formed hair care composition of any suitable ingredients described herein.In embodiment, the present invention includes by polyquaternary ammonium salt-28 and methyl vinyl ether/maleic acid; Approximately 1% to about 5% thickening agent; Approximately 10% or more propylene glycol; And approximately 5% or the more formed hair care composition of emollient, wherein percentage ratio is based on the gross weight meter of compositions.In embodiment, the present invention includes by polyquaternary ammonium salt-28 and methyl vinyl ether/maleic acid; Approximately 3% to about 5% thickening agent; And approximately 2% or the formed hair care composition of emollient still less, wherein percentage ratio is based on the gross weight meter of compositions.In embodiment, the present invention includes by polyquaternary ammonium salt-28 and the formed hair care composition of methyl vinyl ether/maleic acid, wherein the viscosity of compositions is greater than 3000 centipoises.In embodiment, the present invention includes the Emulsion form hair care composition that is formed by polyquaternary ammonium salt-28 and methyl vinyl ether/maleic acid, it has the freeze-thaw stability of improvement with respect to the comparative composition that contains multiple such compound polyelectrolyte.In embodiment, the present invention includes by the formed hair care composition of polyquaternary ammonium salt-28, methyl vinyl ether/maleic acid and polyvinyl pyrrolidone.
The present invention also provides the embodiment of hair nursing preparation and their using method, compares with untreated hair, and it can't increase the needed power of combing hair; Compare with untreated hair, can't increase the needed power of adhesion of separating two hair fibers; Compare with untreated hair, can't increase " three-point bending " power; Compare with untreated hair, can't increase Young's modulus; Compare with untreated hair, can't reduce the brilliance/gloss of hair; Perhaps can not give other quantifiable " negative " attribute.
Compositions of the present invention can any suitable method for the treatment of hair in.For example, can be used for rinsing hair fiber and the conditioning hair fiber by compositions being applied to hair fiber and water in compositions described herein.After rinsing, hair fiber can come with hair-dryer dry, combing and/or finalize the design with approved product or compositions.Additionally, compositions described herein can be used for the furcated end by compositions being applied to furcated end and repairing hair fiber with the water rinse furcated end.Next this method can also dry up, combing and/or typing.Compositions described herein is also to be used for by compositions of the present invention being applied to hair fiber and strengthening the method for hair fiber with this hair of water rinse.In other embodiment, compositions of the present invention can be used for hair fixing, for example when described compositions comprises the hair fixing beneficial agent.For example, compositions can be typing spray (aerosol and non-aerosol).In other embodiment, compositions of the present invention can be used for washing hair with shampoo when being formulated as shampoo.Other approved product can comprise the leave conditioner, the conditioning inorganic agent that spends the night, typing emulsion/ointment/balsam, typing gel, hair styling mousse, essence, hair care oil, polishing material and conditioning spraying (aerosol and non-aerosol).
The freeze-thaw stability of hair care composition that comprises the compound polyelectrolyte of cation type polymer and anionic polymer can be by will approximately 1% being added in hair care composition to about 5% thickening agent and improving, and wherein percentage ratio is based on the gross weight meter of compositions.Thickening agent can comprise quaternary nitrogen compound or polymer.Quaternary nitrogen compound or polymer can be polyquaternary ammonium salt-37 for example.Polyquaternary ammonium salt-37 can be in the mixture with propylene glycol dicaprylate/dicaprate and polypropylene glycol-1 tridecyl alcohol polyethers-6.Perhaps, comprise cation type polymer and anionic polymer compound polyelectrolyte hair care composition freeze-thaw stability can by with approximately 10% or more propylene glycol be added in hair care composition and improve, wherein percentage ratio is based on the gross weight meter of compositions.
The invention provides the heat protection of hair.When the leave compositions that will have PEC described herein was applied to hair, PEC can protect a bar to avoid the damage (for example fiber is cracked) that is caused by heat.Heat can be from any source, for example comprises hair-dryer, ironing board (flat iron) or thermal finalization instrument.
Method of the present invention allows to prepare PEC in a container.Therefore, one aspect of the present invention provides the method for preparing compound polyelectrolyte, and the method is included in the methyl vinyl ether that will have in container as shown in the formula the repetitive of (formula I)/maleic acid hydration
Figure BPA00001701982700291
This methyl vinyl ether/maleic acid is reacted, to form intermediate blend in this container with the alkali (for example sodium hydroxide) that is enough to the amount of at least part of its acidic-group of neutralization; Heating this intermediate blend in this container; Will be as shown in the formula the vinyl pyrrolidone of (formula II)
Figure BPA00001701982700301
With the methacryl amido oxypropyl trimethyl ammonium chloride as shown in the formula (formula III)
Figure BPA00001701982700302
Cationic copolymer be added to intermediate blend in this container; And mix that in this container, multiple polymers prepares compound polyelectrolyte at high shear force and at least about the temperature of 50-60 ℃.
Additionally, another aspect of the present invention allows by PEC prepared in accordance with the present invention is combined to prepare hair care composition with other hair beneficial agent.The method according to this invention, such hair care composition can be by combining PEC prepared in accordance with the present invention to prepare with other hair beneficial agent in single container.Therefore, the present invention also provides and has comprised the method for preparing hair care composition of making compound polyelectrolyte, and it comprises the steps: will to have the methyl vinyl ether of the repetitive of formula I/maleic acid hydration in container; Make this methyl vinyl ether/maleic acid in container be enough to the alkali of the amount of at least part of its acidic-group of neutralization, for example sodium hydroxide (for example 20% sodium hydrate aqueous solution) reaction (for example the alkali by adding capacity is to obtain approximately 6.5 to approximately 7.5 or approximately 6.9 to about 7.0 pH), to form intermediate blend, heat in this container intermediate blend for example to approximately 50 ℃ to the about temperature of 60 ℃; The cationic copolymer of the methacryl amido oxypropyl trimethyl ammonium chloride of the vinyl pyrrolidone of formula II and formula III is added in intermediate blend in this container; And at high shear force and the multiple polymers in for example approximately mixing this container at the temperature of 50-60 ℃ prepare compound polyelectrolyte.Method of the present invention comprises that randomly the other composition that further one or more is selected from aqueous carrier, surfactant, flavouring agent, conditioner, emollient, emulsifying agent, thickening agent, antiseptic, gellant, siloxanes, hair-strengthening agent, wetting agent and wetting agent is added in compound polyelectrolyte in this container; And the compositions of mixing gained in this container.
The present invention also allows to prepare hair care composition in two containers, and PEC prepares in a container and the residual components of compositions prepares in second container, wherein, and then with PEC and other component combination.In this one side, the present invention also provides the method for preparing hair care composition, comprise that the cationic copolymer by methyl vinyl ether/maleic acid and vinyl pyrrolidone and methacryl amido oxypropyl trimethyl ammonium chloride prepares compound polyelectrolyte, it comprises following step: will have the methyl vinyl ether of the repetitive of formula I/maleic acid hydration in the first container; Methyl vinyl ether/maleic acid is reacted with the alkali that is enough to the amount of at least part of its acidic-group of neutralization, for example sodium hydroxide in the first container, to form intermediate blend; Heat the intermediate blend in the first container; The cationic copolymer of the methacryl amido oxypropyl trimethyl ammonium chloride of the vinyl pyrrolidone of formula II and formula III is added to intermediate blend in the first container; The polymer that mixes in the first container at high shear force and at least about the temperature of 50-60 ℃ prepares compound polyelectrolyte; Mix one or more and be selected from the composition of aqueous carrier, surfactant, flavouring agent, conditioner, emollient, emulsifying agent, thickening agent, antiseptic, gellant, siloxanes, hair-strengthening agent, wetting agent and wetting agent in second container; And first or second container in the compound polyelectrolyte of the first container and the blending constituent of second container are mixed.
As mentioned above, can generate the condition of phasor to determine that PEC forms, comprising polymer: polymer weight ratio and electric charge-electric charge ratio.Other condition also can change, and comprises temperature, dicyandiamide solution etc.Can change each effect to determine that they form for PEC in these conditions.Therefore, PEC needs different condition and relates to a large amount of variablees due to preparation, and the preparation of PEC can be complicated and difficulty.Especially in the situation of the specific particle size of expectation, as in preparation can be repaired the PVMMA/ polyquaternary ammonium salt-28PEC of the impaired hair of furcated end.Except polymer: polymer weight ratio and/or electric charge-electric charge ratio etc., the concrete preparation method of using also can affect the mean particle size distribution of PEC.For example, mixing velocity and/or incorporation time in a kind of polymer is added into alternative process, and the mixing velocity after this interpolation and/or incorporation time can affect the PEC particle size distribution.Other process variables, for example the existence of temperature, pH and other charging cpd also may have impact in the PEC forming process.Compositions of the present invention can prepare by the method that allows PEC large-scale production, wherein, can obtain for the appropriate particle size distribution of repairing furcated end.
The formation of PEC can promote by applying heat in the specific stage, for example in alkali and during anionic polymer and/or cation type polymer is being joined anionic polymer when preparing complex.Compositions can be carried out preheating before conjugated polymer, can heat together with a kind of or subgroup of polymer, perhaps can during in conjunction with the polymer of the PEC that is useful on of institute formation or heat afterwards.For PVMMA/ polyquaternary ammonium salt-28PEC, have been found that now the PVMMA that heating has neutralized before adding polyquaternary ammonium salt-28 is favourable, for example at least 50 ℃ to 60 ℃ or larger temperature.Described temperature range is for example as listed in following table.In described table, " X " expression scope " from [respective value the first row] to [respective value in first row] ".For example, first " X " is the scope of " from approximately 50 ℃ to approximately 51 ℃ ".
Table 8
Figure BPA00001701982700321
Therefore, described temperature can have any two scopes that define by aforementioned end points.
Compositions of the present invention can be prepared in single container or can be prepared in the container that separates, and for example PEC and other composition prepare independently, then PEC is being combined with other composition.Method preparation described herein has the PEC of same size, form and stability with conventional method, but does like this quantity that can reduce container.
The step of cation type polymer being added to intermediate blend can comprise that solution, for example aqueous solution with cation type polymer add in intermediate blend.Cation type polymer can be added in intermediate blend with any suitable speed, this can comprise for example per minute for approximately 0.3kg/ minute to per minute for approximately 1.0kg/ minute per minute (for example, if be 10 minutes during adding, speed will be approximately 3kg/ minute to approximately 10kg/ minute so), and for example can comprise listed those in following table.In described table, " X " expression scope " from [respective value the first row] to [respective value in first row] ".For example, first " X " be " from approximately 0.3kg/ minute per minute to approximately 0.4kg/ minute per minute " scope.
Table 9
Figure BPA00001701982700331
Therefore, interpolation can have any two scopes that define by aforementioned end points.
In the time of in a kind of polymer is added into another kind of polymer, mixing velocity and mixed duration are depended in the formation of PEC.Can use high shear force is used for completing mixing.Yet, for suitably forming PEC, may have to regulate mixing velocity according to polymer-polymeric system.For PVMMA/ polyquaternary ammonium salt-28PEC, at first polyquaternary ammonium salt-28 can mix for example 5 minutes, 10 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes or 60 minutes before adding PVMMA.In polyquaternary ammonium salt-28 can being added into PVMMA within the time of for example 5 minutes, 10 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes or 60 minutes.In polyquaternary ammonium salt-28 can being added into PVMMA within the time of 30 minutes.Adding speed can be any suitable speed that forms PEC.Described speed can be determined based on adding the needed time.For example, speed can be based on the addition per minute in during interpolation per minute.For PVMMA/ polyquaternary ammonium salt-28PEC, this can be approximately 0.4kg/ per minute minute to 1.0kg/ per minute minute.Therefore, if be 10 minutes during adding, speed will be approximately 4kg/ minute to approximately 10kg/ minute so.After adding polymer, mixing can continue the time of for example 5 minutes, 10 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes or 60 minutes.Before mixing can be included in interpolation polyquaternary ammonium salt-28, during and/or the combination that mixes afterwards.Therefore, the intermediate blend of PVMMA can be mixed at least about 10 minutes before adding cation type polymer, mix at least about 10 minutes after adding cation type polymer, or its combination.
Some embodiment of the present composition comprises the compositions that has as the preparation of the PVMMA in table 10 and polyquaternary ammonium salt-28.
Table 10
PEC active component % by weight 1% 2% 4% 6% 8%
Water 7.775 15.55 31.1 46.65 62.2
Gantrez AN-119 0.1 0.2 0.4 0.6 0.8
Sodium hydroxide, water (20% active component) 0.125 0.25 0.5 0.75 1
Polyquaternary ammonium salt-28, water (20% active component) 4.5 9 18 27 36
* the residual components * of compositions 87.5 75 50 25 0
Total amount 100 100 100 100 100
The invention provides after PEC forms and the mixing of other composition, wherein, described mixing is enough to allow the abundant combination of one or more compositions.
The invention provides the single vessel process for the preparation of PEC, this is efficiently, cheaply, and eliminated as carry out in conventional PEC preparation method with material required extra time and work from a container is transferred to another container.Therefore, method of the present invention is specially adapted on commercial size, and for example approximately 500 to about 10,000 gallons of preparation PEC and contain the hair care compositions of PEC.
Method of the present invention further provides the PEC compositions for preparing its concentration and significantly surpassed the PEC composition concentration of conventional preparation (being for example 8 % by weight).Concentration when improving preparation PEC has several advantages.Higher concentration allows use less premixing container and PEC is combined with other composition, to make hair care composition, for example conditioner.And, can prepare and store PEC and be used for using in the future, and for more concentrated raw material, need less memory space.In addition, need quality control step still less, because can and test the PEC of batch with higher concentration preparation, rather than prepare a plurality of batches with low concentration, this needs extra test.Additionally, if the PEC raw material is used to prepare hair care composition, the PEC raw material will can not need so many volume in process vessel so, and this allows to add other composition of more volume, and allow to obtain other composition of higher concentration.For example, the applicant has been found that and is preparation PVMMA/ polyquaternary ammonium salt-28PEC, and dilution polyquaternary ammonium salt-28 are (for example, the available Conditioneze NT-20 of business, its concentration is 20% active component) not necessarily.More rightly, according to the present invention, PVMMA/ polyquaternary ammonium salt-28PEC can be prepared by directly undiluted Conditioneze NT-20 being added in the PVMMA copolymer in single container, and this has produced stable high concentration PEC surprisingly.In addition, the applicant has been found that higher PEC relative concentration in compositions prepared in accordance with the present invention is in the conventional PEC compositions of lower concentration, basically more likely with in order to prepare hair care composition, for example other composition of conditioner forms stable Emulsion together.
The invention provides the method for graphical reconstruct repair process in a kind of furcated end repairing hair fiber.In one embodiment, the method comprises hair fiber is fastened to the surface, and the hair fiber that wherein is fastened to described surface has furcated end or be damaged to produce furcated end on this surface the time; Should be associated with multiplying arrangement on the surface, wherein furcated end is placed in the visual field of multiplying arrangement; Image-capturing apparatus is associated with amplifying device, thus the enlarged image in the visual field of seizure multiplying arrangement; Use the compositions-treated furcated end, wherein said composition is repaired furcated end, and wherein this furcated end merges; And by the image-capturing apparatus that is associated with multiplying arrangement, catch the reparation image of furcated end in the compositions-treated process, and store the representative image of the reparation image that catches, be used for retrieval subsequently.Comprise with video according to the method for graphical reconstruct hair of the present invention reparation and come real time record hair repair process.Reason is hoped ground, and the hair repair process uses the video equipment that is applicable to the real time record repair process with the amplification of the repair process that is enough to detect by an unaided eye, and for example carries out record with 20-50 amplification doubly.This video can use method known to those skilled in the art to be stored on recording medium, is used for follow-up retrieval.
Additionally, method of the present invention can comprise hair fiber is fastened to the surface, is fastened to wherein that this surperficial hair fiber has furcated end or damaged to produce furcated end on this surface the time.Therefore, hair fiber can have furcated end before it is fastened to described surface, and perhaps furcated end can be lured formation (for example mechanically) into after hair fiber is fastened to this surface.The surface can be any surface that can be associated with multiplying arrangement.Such surface can comprise for example desktop or microslide.The characteristic on surface can be determined by the type of the multiplying arrangement of using.For example, if use optical microscope, wherein make light pass sample, can use transparent surface, for example microslide so.As another example, the surface can be that hair fiber can be put dressing table thereon.As another example again, if multiplying arrangement is simple lens, magnifier for example, the surface can be desktop so.Should there be anything to interfere the reparation of furcated end.For example, if coverslip will stop the end of furcated end to flock together, should not use the coverslip for microslide.
Hair fiber can be undertaken by any suitable mode fastening, comprises and for example uses one or more fixtures.It is fastening that described hair fiber can also use adhesive tape to carry out, for example, and when using desktop or microslide.As long as the bifurcated of hair fiber can utilize multiplying arrangement to observe, can make in any suitable manner hair fiber fastening (for example fixing) to the surface.
Method of the present invention can comprise described surface is associated with multiplying arrangement, and wherein furcated end is placed in the visual field of multiplying arrangement.Multiplying arrangement can be for example magnifier, microscope (for example optical microscope).Each multiplying arrangement all has the visual field." visual field " refers to the image-region that is used for observation that multiplying arrangement amplifies.Furcated end is placed in the visual field, so that furcated end is exaggerated to be used for observation.
Method of the present invention can comprise image-capturing apparatus is associated with multiplying arrangement, thereby catches the enlarged image of the visual field of multiplying arrangement.Image-capturing apparatus can be numeroscope for example.Image-capturing apparatus can also be simulator.The limiting examples of image-capturing apparatus also comprises photographing unit, video camera, charge-coupled image sensor (CCD) photographing unit, digital camera and/or field camera, perhaps any other similar recording equipment.
Method of the present invention can comprise uses the compositions-treated furcated end, wherein said compositions, repairs furcated end, and wherein furcated end merges.Processing can for example comprise compositions is massaged in hair.Processing can also comprise that for example the rinsing hair to remove compositions, is for example used rinse-off compositions.Can allow compositions to be retained on hair, for example when using the leave compositions.The method of processing can be any suitable method, comprises method described herein.Compositions can be any suitable compositions, comprises compositions described herein.
Method of the present invention can comprise such step: by the image-capturing apparatus that is associated with multiplying arrangement, catch the reparation image of furcated end in the process of processing with described compositions, and the representative image of the reparation image that storage catches is used for retrieval subsequently.Image-capturing apparatus can make the reparation that catches in any suitable manner furcated end.For example, if image-capturing apparatus is numeroscope, numeroscope can produce electronic document so.As another kind of example, if image-capturing apparatus is photographing unit, photographing unit can catch reparation with film so.
The representative image of the reparation image that storage catches is used for later retrieval can be by any suitable mode.For example, this can comprise the electronics representative image of memory image, for example uses addressable electronic document on digital camera and/or computer.This can also be by using film.
In addition, the present invention can be used to be conveyed to any method of consumer.These can comprise and for example use still photo (for example before photo and afterwards); Chart is retouched to and/or schemes; Computer intuitively shows; And/or in the body of use actual human body hair fiber or analog (for example sheep's wool)/external/former digital video.Additionally, the method for reception and registration can be in printing, TV, network, shop, demonstration (for example outpost display) and/or public media in person.Method of the present invention can also be used to explain bonding mechanism (for example PEC shrinks and flocks together with two ends with furcated end).
The present invention also provides qualitative assessment furcated end hair fiber to repair the method for degree, and the method comprises the acquisition wisp of hair, is preferably the hair of twice bleaching; The furcated end of this intrafascicular at least one hair fiber of generation (for example by combing fully and/or dry up this restraint to produce furcated end); Remove at least one hair fiber with furcated end from this bundle; This at least one hair fiber that removes of labelling randomly; Catch the first image of the furcated end of this at least one hair fiber that removes; Make this hair fiber and be associated from the bundle that wherein removes this hair fiber; Should restraint and this hair fiber with compositions-treated; With this hair fiber from this intrafascicular removing; Catch the second image of the end of this hair fiber, wherein this end is the end identical with the first image of the furcated end that is used for catching at least one hair fiber that removes; Numerical value 0 is appointed as furcated end reparation, and 1/2 is that part is repaired, and perhaps 1 is to repair fully; And with the designated value of markd hair fiber add and and with the sum of summation divided by the hair fiber of labelling.When assessing according to this method, the meansigma methods that exemplary composition of the present invention can obtain is for for example being evaluated as 0.85 or larger, for example 0.925,0.95 and or even 0.975 based on 20 fibers.
Method of the present invention can comprise the generation furcated end.This can comprise combing or dry up this bundle hair to produce at least one hair fiber with this bundle of furcated end.Other method comprises selects the nature furcated end.For example, hair sample can obtain from living specimen, and wherein, hair is bifurcated.Yet due to multiformity, this method may cause the repeatability of data poor.
Method of the present invention can comprise the hair fiber that at least one velamen in this bundle hair of labelling removes.Furcated end can be just at the initial part beginning label of bifurcated.If be marked at disappearing after compositions-treated, this can show that furcated end has disconnected hair fiber so.Then, when numerical value was assigned to hair fiber, this root fiber just can be excluded, and also was not repaired because this furcated end has both remained furcated end.Therefore, for example, when the repair ability of evaluation group compound, can avoid false positive.
Method of the present invention can comprise the image of the furcated end of the hair fiber that at least one velamen of seizure removes.The example of such method for catching is described in this article.This step can comprise the electronics representative image of memory image, for example uses addressable electronic document on digital camera and/or computer.
Method of the present invention can comprise with the hair fiber of at least one labelling be associated from the bundle that wherein removes this hair fiber.The hair fiber that removes is returned to this bundle the more natural environment that is used for the repair ability of test composition is provided.Hair fiber and other hair fiber that does not have furcated end with furcated end keep together, and remain in larger hair fiber marshalling.This situation has been simulated normal topknot better, for example the environment on human body head.Remove simply hair fiber with furcated end and the compositions of test on these fibers that remove result based on artificial environment will only be provided.Therefore, when the compositions of testing with the method for consumer, the present invention allows report significant result concerning those consumers, for example reports about repair the result of hair fiber in environment important concerning consumer.
Method of the present invention can comprise the hair fiber of processing this bundle and this at least one labelling with compositions.This processing can for example comprise compositions is massaged in hair.This processing can also comprise that for example the rinsing hair to remove compositions, is for example used rinse-off compositions.Can allow compositions to remain on hair, for example when using the leave compositions.This processing method can be any suitable method, comprises method described herein.Compositions can be any suitable compositions, comprises compositions described herein.
Method of the present invention can comprise the parameter of determining that hair is repaired.The speed of for example, repairing furcated end can in the condition of definition, for example be determined under those conditions described herein.Then compositions can be compared to determine which can provide repairing sooner of furcated end.Use and/or the furcated end remediation efficiency of the compositions of testing can also for example use video method described herein to determine.The reparation of furcated end be preferably 1 hour, be less than 50 minutes, be less than 40 minutes, be less than 30 minutes, be less than 20 minutes, be less than 10 minutes, be less than 5 minutes or be less than in 1 minute.The completeness of repairing or amount can be 10% or larger, 20% or larger, 30% or larger, 40% or larger, 50% or larger, 60% or larger, 70% or larger, 80% or larger, 90% or larger or (for example approximately 100%) fully.Reparation can or be untreated with respect to negative control to measure, and wherein handled furcated end can demonstrate statistically improving significantly in the furcated end reparation (for example the reparation is faster and/or the reparation amount is larger or repair completeness).
Method of the present invention also comprises is appointed as furcated end reparation with numerical value 0, and 1/2 is that part is repaired, and perhaps 1 be to repair fully, and with the appointment numerical value of markd hair fiber add with, and with the sum of summation divided by institute's labelling hair fiber.Therefore, for example when the statistics of all furcated end that have halved tie, the numerical value that obtains will provide the ability of compositions, repairs furcated end.Compositions with poor repair ability will have low and/or approach zero numerical value, and the compositions with better repair ability will have higher and/or close to 1 numerical value.Therefore compositions can contrast with method of the present invention, wherein causes the compositions of higher numerical value that better reparation than the compositions that causes lower numerical value is provided.
Can repair by method of the present invention the furcated end of any type.One type of furcated end comprises for example elementary furcated end.In such furcated end, hair fiber contains the single bifurcated along the hair fiber longitudinal axis, has produced two ends of hair fiber.Another example of furcated end comprises double-Y shaped furcated end, and it is produced by the extra bifurcated along the elementary furcated end longitudinal axis.Tree-shaped furcated end is an example of furcated end, wherein exists several double-Y shaped bifurcateds in a hair fiber.Another example of furcated end is that the end of hair fiber has many penniform short bifurcateds, and it can cause the thickness of fiber axis to change usually.Another example of furcated end is long furcated end, and wherein, a side of elementary furcated end is significantly than opposite side longer (for example a side disconnects).The taper furcated end is another example of furcated end, and wherein only the part of hair fiber remains on end.Furcated end can also be for example quantity by end characterize, for example three furcated end have the hair fiber of two bifurcateds.Degree of depth furcated end is the example (needing not to be end) at the bifurcated of the mid point generation of sending out axle.Slight furcated end is an example that only has the furcated end of slight bifurcated in hair fiber.Term as used herein " furcated end " can comprise the bifurcated of the end that does not extend to hair fiber.The example of such bifurcated is incomplete bifurcated.Fig. 4 A-4D has shown the furcated end of some type.
The hair fiber that uses in the method for the invention can be any mammalian hair.In one embodiment, this hair is the human hair.Can use any country, area or ethnic human hair, for example European, Aisan, African or Caucasian.In one embodiment, this hair is European hair.This hair can have due to for example once bleaching, twice bleaching, the damage of any type of bleaching, dyeing or mechanical failure more than twice.This hair fiber can not have any damage, as original hair.Additionally, the hair form that uses in the method for the invention can be from the method for taking turns be taken turns to another and is changed.The change of this hair can be corresponding to the using and testing of different components, and what it can for example depend on that expectation conveys to consumer is the result of which kind of type.Change the result that hair form and/or compositions will allow to pass on any hair form and any hair care composition.
One aspect of the present invention comprises selects to have the hair fiber of furcated end, and for example cuts into the approximately length of 1-1.5 inch (measuring from the furcated end side).The adhesive tape that can use small pieces is for example to be fastened on described fiber on microscope slide.Microscope slide can be placed on the microscopically that has 50 * amplification for example and be connected with computer with photographing unit.Can correspondingly regulate illumination and focus on.Depend on setting, record can carry out in computer interface, perhaps video camera can be arranged on the spider that for example points to computer screen.By the record of photographing unit, can use micropipettor with a compositions, for example contain 2% activated complex and be applied on furcated end.Can further correspondingly regulate illumination and focus on, can open hair-dryer, for example in heat and aim at furcated end.Can carry out betwixt record, and until furcated end repaired completely or partially.
Another aspect of the present invention comprises and gathers the human hair, is preferably impairedly, most preferably is the European hair of twice bleaching, and is assembled into, and for example uses the band of wax combination, and it can be that for example the 1-1.5 inch is wide.Then with thousands of times of these bundle combings, make simultaneously hair-dryer vertically point to the combing direction to form the furcated end of right quantity.Select the fiber with furcated end of selected quantity (for example 10-20) and extract out from the fiber group.Gather the photo of each fiber ends with 20-50 * amplification by microscope.Pyrite hoop bar is clipped on each fiber and relative end furcated end.Then these pyrite hoop bars are carried out labelling and are placed between two masking tapes.Then this group is inserted into the middle part of topknot, and paper using is clamping fixed to keep this group in appropriate position.Then process a series of circulations of this bundle with washing-off type furcated end remediation composition capable, for example three circulations.After final circulation, fixture is removed and gathers the new photo of furcated end.By before contrast and photo afterwards, the appraiser can provide numerical value " 0 " for repairing, and " 1/2 " be the part reparation, and " 1 " is reparation fully.These numerical value are added and and express divided by the fiber sum degree that furcated end is repaired.
As noted before, use in embodiments of the present invention image capture system with repair or attempt to repair before and generate afterwards the representative image of the outward appearance of furcated end.Although in the scope of this paper instruction, multiple such image capture system can be arranged, exemplary such system is shown in Figure 6.Particularly, Fig. 6 is the schematic diagram of display image data capture system, can carry out therein described picture catching and procedure of processing.
Illustrated system 600 comprises several interactive components, comprises sample support device 601, as is suitable for supporting platform or the surface of sample 602.Sample support device 601 can be transparent throwing light on to allow carrying out the bottom by light source 603.Described light source 603 can also be disposed in bracing or strutting arrangement 601 tops to provide illumination by reflection.
Provide captured electronic image device 604 to be used for catching enlarged image or the video sequence of sample 602 when processing.In this, amplifying device 605 adjacent with sample support device 601, between sample support device 601 and image capture device 604.Image capture device 604 can also be still camera or the video camera that is applicable to catch image sequence.Amplifying device 605 can be for example optical microscope of optical loupes or lens devices, can be perhaps electronic amplifier equipment, such as ultramicroscope etc.In embodiments of the present invention, image capture device 604 and/or amplifying device 605 can be can scan with the zones of different that catches sample 602 or the image of fragment.
Provide auxiliary calculating and data capture device 606 to control and to receive the data from image capture device 604.Auxiliary calculating and data capture device 606 are calculation processing apparatus, and it can receive the electronic image data and control signal is sent to image capture device 604 to catch image from image capture device 604.Described auxiliary calculating and data capture device 606 can also be controlled illuminator 603.
In embodiments of the present invention, will assist calculate and data capture device 606 by wired or wireless, this locality or remotely communicate to connect to electronic databank 607.In this way, auxiliary calculate and data capture device 606 can from image capture device 604 collect data and electronic databank 607 the collected data of storage be used for subsequently analysis, control and/or relay, for example to printing or publication device (not shown).
Described auxiliary calculating and data capture device 606 can be computers, such as PC, portable computer, work station etc., and carry out by computer the computer-readable instruction that is stored on computer-readable medium and operate.Computer-readable medium is tangible medium, for example disk or optical disk system, flash disk, PRO etc.Therefore, the step that relates to data capture, controls and/or transmit discussed in this article is carried out by this way.User interface 608 allows users to receive in human understandable mode to come from auxiliary calculating and the information of data capture device 606, and provides in the intelligible mode of computer and input to described device.In embodiments of the present invention, user interface 608 comprises graphic user interface and keyboard, button, pincushion, mouse and/or other the user's input mechanism on screen.
In embodiments of the present invention, described image capture device for example comprises the video camera of the reparation situation of sending out axle of one or more furcated end for being applicable to one or more axles of real time record.Ideally, described video carries out record under the amplification that is enough to bore hole Real Time Observation hair repair process.Suitable amplification can comprise 20-50 for example * amplification.
The following examples have further described the present invention, but certainly should not be interpreted as limiting the scope of the invention by any way.
Embodiment 1
The present embodiment has illustrated that the method with twin containers prepares the hair care composition that comprises compound polyelectrolyte.
Compositions 1A-1C
Figure BPA00001701982700431
Figure BPA00001701982700441
For listed blender in the present embodiment and other embodiment, those skilled in the art can be based on determining particular container to be used and determining that according to listed experimental program appropriate RPM sets.
In suitable, rustless steel pre-mix reservoir, the water that is filled with is set as 113-131 ℉ (45-55 ℃).(turbine-type mixer is with strong clockwise direction to begin strong turbine mixing; Side is swept blender and is closed).In case batch temperature reaches 86 ℉ (30 ℃) or higher, and under strong mixing, with the PVMMA copolymer (
Figure BPA00001701982700442
S-97BF; ISP, Wayne, NJ, USA) be added into lentamente pre-mix reservoir.Correspondingly regulate to mix and can not produce excess foam on liquid surface to obtain strong stirring.In case all powder all add, use the water that is set as 113-131 ℉ (45-55 ℃) to come rinsing hybrid blade and sidewall.In case rinsing is completed, open side is swept agitator and is begun to be heated to 122-131 ℉ (50-55 ℃).(powder agglomates will disperse faster when premix is combined into 113-131 ℉ (45-55 ℃)).Continue heating and keep this temperature between whole mixing period.(turbine-type mixer is with strong counter clockwise direction to set blender; Side is swept blender with moderate clockwise direction).
Mixed this batch of material at least 20 minutes, perhaps until do not have granule or piece.
In case premixing evenly and not contains piece, reduce turbine and be mixed to moderate degree.Sodium hydroxide is added into pre-mix reservoir and mixed 10 minutes.Described solution will have low viscosity and will occur slight muddiness that (blender setting: turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction).Mixed described batch of material at least 10 minutes or until fully even.
In case described batch of material is uniformly, sample is carried out in-process pH test.Continue the retest sample, until obtain the stable pH reading of 6.9-7.0.If pH is low, additionally add 20% sodium hydroxide with scope up to specification.Again mix also sub-sampling again.If pH is high, additionally add aspartic acid with scope up to specification.Again mix also sub-sampling again.
In case Gantrez is by hydration and pH in specification, check whether the premixing temperature is 122-131 ℉ (50-55 ℃) fully.Heat in case of necessity.In case premix is combined into 122-131 ℉ (50-55 ℃), to close side and sweep agitator, counter-rotating turbine direction also improves the turbine mixing velocity (turbine-type mixer is with strong clockwise direction to produce eddy current; Side is swept blender and is closed).
Add lentamente polyquaternary ammonium salt-28 ( NT-20 (20% active component); ISP, Wayne, NJ, USA) to pre-mix reservoir.Slowly adding in the pre-mix reservoir is for obtaining suitable compound polyelectrolyte particle size.Adjust the interpolation flow rate with the drum spout.Whole open containers once is not poured onto in the premixing container.In the adding procedure of this material, described premixing will become unusual thickness, and begin to bleach.In case all materials add, solution will dilute and show as in appearance the Lac Bovis seu Bubali shape again.
Counter-rotating turbine direction and open side are swept agitator.Mixed consumingly 20 minutes or until premix fully evenly (turbine-type mixer is with strong counter clockwise direction, and side is swept blender with moderate clockwise direction).Mix described batch of material at least 20 minutes or until do not have visible granule or piece.
In case complete described mixing, the described premix of collected specimens and visual observation.Check that it has been hololeucocratic and has not had muddy or gloomy.Check that also described premix viscosity is rare and the Lac Bovis seu Bubali shape and can be too not sticking.If described premix is not rare and Lac Bovis seu Bubali shape, continue to mix consumingly extra 20 minutes and sub-sampling again.
In case described premix is fully even, weakens and stir and begin to cool down, to 86-113 ℉ (30-45 ℃).In main clad vessel, (turbine-type mixer is with moderate counter clockwise direction until described pre-composition is about to be added to keep mixing and temperature; Side is swept blender with moderate clockwise direction).
In the compound container of main rustless steel, the water that is filled with is set in 180-185 ℉ (82-85 ℃), and (turbine-type mixer is with moderate counter clockwise direction under moderate mixing; Side is swept blender with moderate clockwise direction).Lentamente EDETATE SODIUM and aspartic acid are added in main clad vessel.After component is added, begin to heat batch of material to 180-185 ℉ (82-85 ℃), (turbine-type mixer is with moderate counter clockwise direction) as required.Continue the described batch of material of heating to 180-185 ℉ (82-85 ℃).Mix the described batch of material time of at least 5 minutes or until solid dissolve fully.
In case batch temperature is 176 ℉ (80 ℃) or higher, SAPDMA is added in main clad vessel, and mix until its complete melting (turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction).Continue the described batch of material of heating to 180-185 ℉ (82-85 ℃).Mixed described batch of material at least 5 minutes or until the complete melting of solid.
In case batch temperature is 180-185 ℉ (82-85 ℃), just following component is added into main clad vessel: the spermol, stearyl alcohol, glyceryl stearate and the PPG-3 benzyl oxide myristinate that are used for compositions 1A (conditioner); The spermol, glyceryl stearate and the aminopropyl polydimethylsiloxane that are used for compositions 1B (cream spends the night); The spermol and the glyceryl stearate that are used for compositions 1C (leave cream).In case batch temperature is 180-185 ℉ (82-85 ℃) again, (turbine-type mixer was with moderate counter clockwise direction at least 30 minutes to keep this temperature and mixing; Side is swept blender with moderate clockwise direction).Keep it when mixing described batch of material between 180-185 ℉ (82-85 ℃).
From main clad vessel collected specimens and all meltings of solid of visual examination, and described batch of material is smooth and uniform.If have any undissolved material or granule, continue strong the mixing, and sub-sampling again.
Begin to cool down described batch of material to 104-113 ℉ (40-45 ℃), and reduce turbine and side sweep agitator speed to moderate/slowly degassed (turbine-type mixer is with moderate counter clockwise direction to help described batch of material; Side is swept blender with slowly clockwise).In case during cooling batch temperature is 167 ℉ (75 ℃) or when lower, (turbine-type mixer is with moderate counter clockwise direction propylene glycol to be added into main clad vessel; Side is swept blender with moderate clockwise direction).For compositions 1C (leave cream), also add glycerol under this mixing velocity.
In a single day main batch temperature is 150 ℉ (65 ℃) or lower for compositions 1A (conditioner), be in a single day perhaps 131 ℉ (55 ℃) or lower for cream, close side and sweep agitator, the direction of counter-rotating turbine stirrer, and (turbine-type mixer is with moderate clockwise direction to produce slight eddy current to strengthen mixing; Side is swept blender and is closed).Will
Figure BPA00001701982700471
SC-96 (the propylene glycol dicaprylate/dicaprate of 65% polyquaternary ammonium salt-37,25%, 10% PPG-1 tridecyl alcohol polyethers-6; Ciba/BASF, Basel, Switzerland) be added into main clad vessel, and continue to be cooled to 104-113 ℉ (40-45 ℃).(mixed well in its container before being added into described batch of material
Figure BPA00001701982700472
SC-96).
In case all materials have been incorporated in batch of material and no longer had been positioned at the surface when upper, reverse turbine stirrer and open side are swept agitator (turbine-type mixer are with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction).
In a single day main batch temperature is 150 ℉ (65 ℃) or lower for compositions 1A (conditioner), be in a single day perhaps 131 ℉ (55 ℃) or lower for compositions 1B (cream spends the night), and premix is ready to, described premix is added in main clad vessel.When premix is added, minimize inflation thereby close turbine-type mixer or it is decelerated to slowly so that liquid level surpasses the top setting of turbo blade.In case described premix adds, come rinsing premixing container with the water that is set in 77-95 ℉ (25-35 ℃), and it is added into main clad vessel.Along with premix being mixed in described batch of material, the viscosity of batch of material will reduce.Correspondingly (turbine-type mixer is with moderate counter clockwise direction to avoid splashing for adjusting mixer speed; Side is swept blender with moderate clockwise direction).
For compositions 1A (conditioner), batch mixture at least 15 minutes or until described batch of material is even.In case main batch temperature is 122 ℉ (50 ℃) or lower, Lluid Blend is added directly to main clad vessel.Fully mix in adding procedure.(turbine-type mixer is with moderate counter clockwise direction to sneak into siloxanes to strengthen as required mixing; Side is swept blender with moderate clockwise direction).
For cream, in case all premixs add, if possible, add the water that is set in 77-95 ℉ (25-35 ℃), this lower face at batch of material carries out minimizing inflation.Mixed described batch of material at least 15 minutes or until described batch of material is even.Continue to be cooled to 104-113 ℉ (40-45 ℃).In suitable rustless steel phase vessel or container, the following silicone component of premixing under strong stirring: be used for compositions 1B's (cream spends the night)
Figure BPA00001701982700481
OSW 5 (84% cyclopentasiloxane, 15% dimethiconol, 1% polydimethylsiloxane) and polydimethylsiloxane (60,000cst); Be used for compositions 1C (leave cream) polydimethylsiloxane (60,000cst), the poly-trimethicone (DC-556 of phenyl; Dow Corning) and D5 dimethiconol (DC-1501).In case described siloxanes premix is even, it is added into main clad vessel, and allows the siloxanes pre-mix reservoir to be expelled to as much as possible in main batch of material container.(turbine-type mixer is with on strong counter clockwise direction to sneak into siloxanes to strengthen as required mixing; Side is swept blender with moderate clockwise direction).
When described batch temperature is 113 ℉ (45 ℃) or when lower, following component is added into main clad vessel: flavouring agent (spice), DMDM Hydantoin, Cocoa Cortex cocois radicis oil, keratin aminoacid, flower/leaf extract.For compositions 1B (cream spends the night), also add DC-8500 (82% pair of (C13-15 alkoxyl) PG-ammonia end polydimethylsiloxane, 18%C14-15 alcohol; Dow Corning, Midland, MI, USA).Continue to mix and be cooled to 95-104 ℉ (35-40 ℃).
Mixed consumingly at least 45 minutes or until all cakings remove, and batch of material is smooth and uniform.Described batch of material can be by passing through 80 order filters and recirculation with this final mixture, to help broken caking.Although need to shear (mixing of reinforcement and/or recirculation) with cracked described caking, (turbine-type mixer is with strong counter clockwise direction also will to minimize as far as possible inflation; Side sweep blender with moderate clockwise).At least mixed 45 minutes.
When batch temperature is 95-104 ℉ (35-40 ℃), analytic sample.Stop mixing and cooling.
Can followingly regulate.If pH is low, 5% interpolation sodium hydroxide (20%) take maximum as whole batch of material demands.Again mix also sub-sampling again.If pH is high, 7.5% interpolation aspartic acid take maximum as whole batch of material demands.Again mix also sub-sampling again.If viscosity is low, additionally mixed 60 minutes and sub-sampling again.Batch of material can also pass through 80 order filter recirculatioies.
Should comprise air film type and positive displacement formula for the pump that material is pumped into container.The filter that should use comprises 80 orders for all conveying operations.Filling temp should be 90-99 ℉ (32-37 ℃).If products temperature is reduced to lower than 90 ℉ (32 ℃), do not need to heat again batch of material.
Compositions 1D
Figure BPA00001701982700491
In the compound container of main rustless steel, the water that is filled with is set in 95-104 ℉ (30-35 ℃), and (if feasible, turbine-type mixer is with strong counter clockwise direction to begin strong stirring; Side is swept blender with moderate clockwise direction).Heating water does not come holding temperature.Add lentamente in order following component to the main clad vessel, and mix consumingly that (if feasible, turbine-type mixer is with strong counter clockwise direction; Side is swept blender with moderate clockwise direction) 10 minutes or until fully evenly and not there is piece in batch of material: Gantrez AN-119 (Oantrez S97BF), NaOH, polyquaternary ammonium salt-28 (Conditioneze).Mixed described batch of material at least 10 minutes or until fully evenly and not there is piece in described batch of material.
(if feasible, turbine-type mixer is with strong counter clockwise direction under strong mixing; Side is swept blender with moderate clockwise direction), following component is added in main clad vessel: PVP, EDETATE SODIUM.Mixed described batch of material at least 15 minutes or until solid dissolves fully and described batch of material is even.
After mixing, do not have piece or granule from main clad vessel collected specimens and inspection, and described batch of material is smooth and uniform.If have piece or granule, continuation mixing and sub-sampling again are until described batch of material is smooth and uniform.
(if feasible, turbine-type mixer is with strong counter clockwise direction under strong stirring; Side is swept blender with moderate clockwise direction) begin to heat described batch of material to 170-175 ℉ (76-79 ℃).In case batch temperature reaches 150 ℉ (65 ℃) or higher, just following component is added into main clad vessel: the stearyl dimethyl benzyl ammonium chloride.Keep it between 170-175 ℉ (76-79 ℃) when mixing described batch of material.Mixed described batch of material at least 60 minutes.
Do not have piece or granule from main clad vessel sampling and visual examination, and described batch of material is uniform.If have piece or granule, continue to mix also consumingly sub-sampling again, until described batch of material is even.
Slow down and be stirred to that moderate (if feasible, turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction), and begin to cool down described batch of material to 90-95 ℉ (32-35 ℃).
In cooling, in order following composition is added into main clad vessel.Fully mix after each the interpolation: the cationic Emulsion of DC949; Glycerol USP VEG; The PEG-12 polydimethylsiloxane; Propylene glycol; Triethanolamine; Citric acid.
In case batch temperature is 113 ℉ (45 ℃) or lower, just in order following composition is added into main clad vessel: DMDM Hydantoin; Hydrolyzed silkworm silk albumen; Vitamin mixtures; Polyglycereol-3 distearate mixture.
In the independent stainless steel ware that is equipped with electronics or air mixer or container, the component that premixing is following: polysorbate20; Flavouring agent.This pre-composition of blend consumingly, until the dissolving of all flavouring agents, and described premix is all even transparent.This pre-composition is loaded into main clad vessel under moderate stirring.With the cold rinse premixing vessel/container that is set in 60-80 ℉ (15-27 ℃), and be added in main clad vessel.(if feasible, turbine-type mixer is with moderate counter clockwise direction in mixing; Side is swept blender with moderate clockwise direction) at least 20 minutes or until described batch of material is fully even.
Can followingly regulate.If pH is low, add triethanolamine solution with the increment of 0.20% solution.If pH is high, add citric acid solution with the increment of 0.20% solution.
Should comprise air film type and positive displacement type for the pump that material is pumped into container.The filter that should use comprises 80 orders for all conveying operations.Filling temp should be ambient temperature.Batch of material can be cooling to promote filling as required.
Compositions 1E
Figure BPA00001701982700511
Figure BPA00001701982700521
In the compound container of main rustless steel, in the situation that feasible, add the water that is set as 68-86 ℉ (20-30 ℃), and (turbine-type mixer is with strong counter clockwise direction to begin strong stirring; Side is swept blender with moderate clockwise direction).
Lentamente following component is added in order main clad vessel and mixes consumingly that (turbine-type mixer is with strong counter clockwise direction; Side is swept blender with moderate clockwise direction) 5 minutes or until fully evenly and not there is piece in batch of material: Gantrez AN-119 (Gantrez S97BF), sodium hydroxide (20%), polyquaternary ammonium salt-28 (Conditioneze).Mixed described batch of material at least 5 minutes or until fully evenly and not there is piece in described batch of material.
In case batch of material is even, lentamente following component is sprayed in main clad vessel: Polyquaternium-10.In the situation that possible, use strong mixing to obtain eddy current.(turbine-type mixer is with strong counter clockwise direction with the inboard of the described container of water rinse and blender blade; Side is swept blender with moderate clockwise direction).
Begin to heat described batch of material to 113-122 ℉ (45-50 ℃).Mixed at least 20 minutes in heating, perhaps until polymer by hydration fully, and solution is transparent and uniform.
After mixing, taking a sample from main clad vessel and checking does not exist piece or granule, and batch of material is smooth and uniform.If have piece or granule, continue to mix also sub-sampling again, until batch of material is smooth and uniform.(turbine-type mixer is with moderate counter clockwise direction to slow down the stirring of turbine when continuing heating; Side is swept blender with moderate clockwise direction), and add in order extremely main clad vessel of following component: cocamido propyl betaine, EDETATE SODIUM, citric acid, USP.Mixed at least 10 minutes or until batch of material evenly and all components dissolve fully.
Check that batch temperature is 113-122 ℉ (45-50 ℃).Then, (turbine-type mixer is with moderate counter clockwise direction in order following component to be added into main clad vessel under moderate stirring; Side is swept blender with moderate clockwise direction).Careful operation is to avoid inflation, the mixing and if necessary words slow down: sodium laureth sulfate in adding procedure; The laureth disodium sulfosuccinate; Glycol distearate, cocamido propyl betaine, coconut oleoyl amine MEA, aqueous mixtures; PEG-6 caprylic/capric triglyceride.Rising along with liquid level in container, at liquid level during near blade, the speed that reduces turbine-type mixer is to slowly.In case described blade is covered fully by batch of material, the speed raising with turbine-type mixer is back to moderate.This will help to reduce the inflation of batch of material.Keep it in batch mixture between 113-122 ℉ (45-50 ℃).Mixed at least 20 minutes or until batch of material be smooth and complete uniformly.
Sweep to be stirred to and slowly make batch of material degassed (turbine-type mixer is with counterclockwise slowly by weakening turbine and side; Side is swept blender with slowly clockwise), and begin to cool down described batch of material to 95-104 ℉ (35-40 ℃).
In case batch temperature is 113 ℉ (45 ℃) or lower, the stirring of turbine and side being swept is increased to that moderate (turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction), and in order following component is added into main clad vessel: flavouring agent; Methylchloroisothiazandnone, Methylisothiazolinone, aqueous mixtures; Oleum Cocois; Keratin aminoacid, flower extract.
In independent stainless steel ware or container, mixed chlorinated sodium and be set in 95-104 ℉ (35-40 ℃) water is until this salt disperses fully.Described salt may not can dissolve fully, because the amount of water may be not enough.Be mixed to that described salt disperses fully and then continue.
In case be ready to the premixing of described salt, it be added into main clad vessel and mix, (turbine-type mixer is with moderate counter clockwise direction until described batch of material is fully even; Side is swept blender with moderate clockwise direction).Come the premixed vessel of rinsing or container with cold water, and rinse transmission line.This rinsing/flushing water is added into main clad vessel.Mixed at least 30 minutes or until described batch of material is fully even.Described compositions is taken a sample.Stop mixing and cooling (if feasible).
Can followingly regulate.If viscosity is low, add sodium chloride.Total sodium chloride levels in preparation does not surpass 2.00%.If viscosity is high, add propylene glycol.If pH is low, add sodium hydroxide (20%).If pH is high, add citric acid.
The batch of material of inflation: again heat batch of material to 120-125 ℉ (48-52 ℃), and mixed lentamente 20 minutes.Cool back to 95-100 ℉ (35-38 ℃), add 10% antiseptic, and if necessary words are added flavouring agent.
Should comprise air film type and positive displacement type for the pump that material is pumped into container.The filter that should use comprises 80 orders for all conveying operations.Filling temp should be 90-100 ℉ (32-38 ℃).Batch of material can be heated to this temperature range to help to promote filling.
Compositions 1F
Figure BPA00001701982700551
Before being weighed and being added into batch of material, fully mix in its container
Figure BPA00001701982700552
SC-96.
In suitable, rustless steel pre-mix reservoir, the water that is filled with is set in 113-131 ℉ (45-55 ℃).(turbine-type mixer is with strong clockwise direction to begin strong turbine mixing; Side is swept blender and is closed).
In case batch temperature is 86 ℉ (30 ℃) or higher, and under strong mixing, Gantrez AN-119 (Gantrez S-97BF) is added in pre-mix reservoir lentamente.Correspondingly regulate and mix to obtain strong stirring, and can not produce excessive foam on liquid surface.In case all powder add, use the water that is set in 113-131 ℉ (45-55 ℃) to come rinsing hybrid blade and sidewall.In case rinsing is completed, open side is swept agitator (turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction), and begin to be heated to 122-131 ℉ (50-55 ℃).When premix is 113-131 ℉ (45-55 ℃), powder mass will disperse sooner.Continue heating and keep this temperature between whole mixing period.Batch mixture at least 20 minutes or until do not have granule or piece.
In case premix evenly and not contains piece, slow down turbine and be mixed to that moderate (turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction).Sodium hydroxide is added into the premixing container and mixed 10 minutes.This solution will have low viscosity and will show slight muddiness.Batch mixture at least 10 minutes or until fully even.
In case batch of material is even, sample is carried out in-process pH test.Continue the described sample of retest until obtain stable pH reading.If pH is low, add extra sodium hydroxide (20%) with scope up to specification.Again mix also sub-sampling again.If pH is high, add aspartic acid with scope up to specification.Again mix also sub-sampling again.
In case hydration and pH in regulation, check that the premixing temperature is 122-131 ℉ (50-55 ℃) to Gantrez fully.If necessary heat.
In case premix is 122-131 ℉ (50-55 ℃), to close side and sweep agitator, counter-rotating turbine direction also improves the turbine mixing velocity (turbine-type mixer is with moderate clockwise direction to produce eddy current; Side is swept blender and is closed).Polyquaternary ammonium salt-28 (Conditioneze NT-20) is added into the premixing container lentamente.Be added into lentamente the premixing container to obtain suitable composite particles size.This interpolation should spend 10-15 minute and complete.Adjust the interpolation flow rate with the drum spout.Whole open containers once is not poured onto in the premixing container.
In this Material Addition process, premix will become very sticking and begin to bleach.In case all materials add, described solution just will dilute and show as in appearance the Lac Bovis seu Bubali shape again.
Counter-rotating turbine direction and open side are swept agitator, and (turbine-type mixer is with strong counter clockwise direction; Side is swept blender with moderate clockwise direction).Mixed consumingly 20 minutes or until premix is fully even.Batch mixture at least 20 minutes or until do not have granule or piece.Complete in case mix, sampling and the described premix of visual examination.Check that it has been hololeucocratic and not muddy or gloomy.Check that also described premix viscosity is rare and Lac Bovis seu Bubali shape, and excessive thickness.If described premix is not rare and Lac Bovis seu Bubali shape white, continue to mix consumingly extra 20 minutes and sub-sampling again.
In case premixing is fully even, (turbine-type mixer is with moderate counter clockwise direction to slow down stirring; Side is swept blender with moderate clockwise direction), and begin to cool down to 86-113 ℉ (30-45 ℃).Keep mixing and temperature until premix is ready to and will be added into main clad vessel.
In the compound container of main rustless steel, be filled with the water that is set in 180-185 ℉ (82-85 ℃), (turbine-type mixer is with moderate counter clockwise direction under moderate mixing; Side is swept blender with moderate clockwise direction).
Following component is added into main clad vessel lentamente: EDETATE SODIUM; Aspartic acid.After described component is added, begin as required to heat batch of material to 180-185 ℉ (82-85 ℃).(turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction).Continue the heating batch of material to 180-185 ℉ (82-85 ℃).Batch mixture at least 5 minutes or until solid dissolve fully.
In case batch temperature is 176 ℉ (80 ℃) or higher, SAPDMA be added into main clad vessel and mix, until its complete melting (turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction).Continue the heating batch of material to 180-185 ℉ (82-85 ℃).Batch mixture at least 5 minutes or until the complete melting of described solid.
In case batch temperature is 180-185 ℉ (82-85 ℃), following component is added into main clad vessel: spermol, glyceryl stearate, aminopropyl polydimethylsiloxane.
In case batch temperature is 180-185 ℉ (82-85 ℃) again, keep this temperature and mix 30 minutes that (turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction).Keep it when mixing described batch of material between 180-185 ℉ (82-85 ℃).Mixed described batch of material at least 30 minutes.
After heat was mixed, whether melting and batch of material were smooth and uniform from main clad vessel sampling and all solid of visual examination.If any undissolved material or granule are still arranged, continue strong mixing and sub-sampling more periodically, until all waxs and all dissolved and described batch of material is even.
After heat is mixed, begin to cool down batch of material to 104-113 ℉ (40-45 ℃), and slow down turbine and side sweep agitator speed to moderate/slowly degassed (turbine-type mixer is with moderate counter clockwise direction to help batch of material; Side is swept blender with slowly clockwise).
In case in cooling and batch temperature be 167 ℉ (75 ℃) or lower, (turbine-type mixer is with moderate counter clockwise direction propylene glycol to be added into main clad vessel; Side is swept blender with moderate clockwise direction).
In case main batch temperature is 150 ℉ (65 ℃) or lower, to close side and sweep agitator, (turbine-type mixer is with moderate clockwise direction to produce slight eddy current for the direction of counter-rotating turbine stirrer and reinforcement mixing; Side is swept blender and is closed).Will
Figure BPA00001701982700571
SC-96 is added into main clad vessel and continues to be cooled to 104-113 ℉ (40-45 ℃).
In case all materials are incorporated in batch of material, and no longer be positioned on the surface, reverse turbine stirrer and open side are swept agitator (turbine-type mixer are with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction).
In case main batch temperature is 131 ℉ (55 ℃) or lower, and the PEC active pre-mixture is ready to, and premix is added into main clad vessel.When premix is added, closes turbine-type mixer or slow down it to slowly, to minimize inflation when arranging at the top of liquid level process turbo blade.
In case premix adds, namely use and be set as the cold rinse premixing container of 77-95 ℉ (25-35 ℃), and it is added into main clad vessel.Along with PEC active component premix is mixed in batch of material, the viscosity of batch of material will reduce.Correspondingly (turbine-type mixer is with moderate counter clockwise direction to avoid splashing for adjusting mixer speed; Side is swept blender with moderate clockwise direction).
In case all PEC active component premixs add, if possible, be filled with the cold water that is set as 77-95 ℉ (25-35 ℃) under the surface of batch of material, it minimizes inflation.Mixed described batch of material at least 15 minutes or until described batch of material for uniformly.Continue to be cooled to 104-113 ℉ (40-45 ℃).
In suitable rustless steel phase vessel or container, the following component of premixing under strong stirring: cyclopentasiloxane mixture; Polydimethylsiloxane.In case premix is uniformly, it is added into main clad vessel and allows the premixing container to be expelled to as much as possible that in main batch of material container, (turbine-type mixer is with strong counter clockwise direction; Side is swept blender with moderate clockwise direction), strengthen as required mixing to sneak into siloxanes.
When batch temperature is 113 ℉ (45 ℃) or when lower, following composition is added in main clad vessel: DC-8500; Flavouring agent; DMDM Hydantoin, Oleum Cocois, keratin aminoacid, flower extract mixture.Continue to mix and be cooled to 95-104 ℉ (35-40 ℃).
(turbine-type mixer is with strong counter clockwise direction in mixing consumingly; Side is swept blender take moderate clockwise direction) at least 45 minutes or until all pieces have removed and batch of material as smooth and uniform.Batch of material can pass through 80 order filter recirculatioies in whole this final mixing, to help cracked.Although should use shearing (strengthen and mix and/or recirculation) with cracked described, minimize as far as possible inflation.Mixed at least 45 minutes.When batch temperature is 95-104 ℉ (35-40 ℃), compositions is taken a sample.Stop mixing also cooling.
Can followingly regulate.If pH is low, the 5% interpolation sodium hydroxide (20%) that needs take maximum as total batch of material.Again mix also sub-sampling again.If pH is high, the 7.5% interpolation aspartic acid that needs take maximum as total batch of material.Again mix also sub-sampling again.If viscosity is low, mixed extra 60 minutes and sub-sampling again.Batch of material can also follow bad by 80 order filters again.
Should comprise air film type and positive displacement type for the pump that material is pumped into container.The filter that should use comprises 80 orders for all conveying operations.Filling temp should be 90-99 ℉ (32-37 ℃).If product temperature is brought down below 90 ℉ (32 ℃), need not again heat batch of material.
Embodiment 2
The present embodiment has illustrated and has used single container technique preparation to comprise the hair care composition of compound polyelectrolyte.
The method of embodiment 1 has been described twin containers technique, and wherein compound polyelectrolyte is prepared in a container, and remaining component is mixed in independent container, and compound polyelectrolyte and remaining component are merged.For described method is reduced to a container, the method is carried out as described in Example 1, and difference is at first compound polyelectrolyte is prepared in described container, and other component is added directly to same container after compound polyelectrolyte forms.The final viscosity of described compositions may be lower such as fruit preparation in two containers.In order to compensate, add extra SC 96.
Embodiment 3
The present embodiment has illustrated the compatibility of compound polyelectrolyte (PEC) with some charging cpd and polymer.
Visual appearance: PEC visual appearance in containing the solution of charged particle is characterized.When PVMMA and polyquaternary ammonium salt-28 separate solvent are in water, described compositions is for clarification.When the PEC in water existed with solvation PVMMA and polyquaternary ammonium salt-28, described compositions became muddiness and/or Lac Bovis seu Bubali shape in appearance.After the another kind of charge species that will be in water produces the clarification compositions during solvation is added into PEC, the opacity reduction (and becoming in some cases clarification again) of expection Lac Bovis seu Bubali shape/muddiness.This is the vision indication of PEC combination process counter-rotating.The opaque outward appearance of Lac Bovis seu Bubali shape of 1 % by weight and 2 % by weight PVMMA/ polyquaternary ammonium salt-28PEC greater than 0.5 % by weight polyquaternary ammonium salt-4 (
Figure BPA00001701982700592
L-200; Akzo Nobel, Amsterdam, Netherlands) existence under can disappear.This structure that shows PEC is destroyed.Less than 0.5 % by weight During L-200, PEC can be not destroyed.0.5 % by weight H-100 can not destroy PEC.
Figure BPA00001701982700595
L-200 and H-100 are similarly, but L-200 has lower viscosity and the cation activity of Geng Gao.
Thickening: the Tinovis GTC/ acrylate in the compositions that contains or do not contain PEC/behenyl alcohol polyethers-25 methacrylate copolymer (2.3%) is tested.The compositions that does not contain PEC provides 40,000-60, the viscosity of 000 centipoise.The compositions that contains PEC is water-reducible.Because Tinovis is association thickener, and the compositions that does not contain PEC can by thickening, not become invalid so think Tinovis to be subjected to PEC.
Furcated end is repaired: table 11 has shown charging cpd and the polymer of being combined with PEC.These compositionss do not demonstrate the illeffects that furcated end is repaired.
Table 11
Figure BPA00001701982700601
Embodiment 4
The present embodiment has been described the system that comprises compound polyelectrolyte and electropolymer.
All compositions 4B-4E show freeze-thaw stability.The inventor also finds surprisingly with respect to compositions 4B, 4C and 4E, comprises
Figure BPA00001701982700611
The compositions 4D of SC 96 shows excellent long-term controlled viscosity (wherein said viscosity maintains a long-term stability).
Comparative composition 4A does not comprise PEC, and compositions 4B-4E comprises PVMMA: polyquaternary ammonium salt-28PEC and charging cpd and/or polymer.All compositionss are the washing-off type conditioner.If necessary, regulate to obtain suitable pH with sodium hydroxide/citric acid/aspartic acid.
" MS " identifier standardization.
Compositions 4A-4E
Figure BPA00001701982700621
Goal standard 4A:
pH:4.00-5.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃):
Bulk viscosity: 5,000-9,000 centipoise
W/ shear viscosity (finished product): 10,000-30,000 centipoise
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: viscosity, opaque Emulsion
Goal standard 4B:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃):
Bulk viscosity: 7,000-15,000 centipoise
W/ shear viscosity (finished product): 20,000-35,000 centipoise
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: viscosity, opaque Emulsion
Goal standard 4C:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃):
Bulk viscosity: 7,000-15,000 centipoise
W/ shear viscosity (finished product): 20,000-35,000 centipoise
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: viscosity, opaque Emulsion
Goal standard 4D.
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃):
Bulk viscosity: 7,000-15,000 centipoise
W/ shear viscosity (finished product): 20,000-35,000 centipoise
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: viscosity, opaque Emulsion
Goal standard 4E:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃):
Bulk viscosity: 7,000-15,000 centipoise
W/ shear viscosity (finished product): 20,000-35,000 centipoise
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: viscosity, opaque Emulsion
Embodiment 5
The present embodiment has illustrated the method for the compositions of Preparation Example 4.
For comparative composition 4A, the beginning heating container is to 80-85 ℃ and add following composition: deionized water, citric acid and EDETATE SODIUM.Check that temperature is 80-85 ℃ and adds following composition: quaternary ammonium salt-18/ water, SAPDMA, spermol and stearyl alcohol.Mixed consumingly under 80-85 ℃ 30 minutes.Cooling mixture.Under 57-60 ℃, add lentamente L-Aspartic acid.At 45 ℃ or lower temperature, add following composition: isostearoyl amine propyl group ethyl Dimethyl Ammonium sulfovinate/PEG-9, cyclopentasiloxane/cyclohexasiloxane/polydimethylsiloxane, flavouring agent and DMDM Hydantoin.
Compositions 4B, 4C and 4E prepare with biphase.For compositions 4B, add the deionized water of (compositions final total weight %'s) 52.05 % by weight in principal phase.Begin to be heated to 80-85 ℃.Once add following a kind of composition and mixing until dissolving and the solution clarification that becomes fully: EDETATE SODIUM and L-Aspartic acid.Add following a kind of composition next time and mix until melting at 80-85 ℃: SAPDMA (checking to guarantee that solution becomes clarification), spermol and tristerin.Mixed consumingly under 80-85 ℃ 30 minutes.After 30 minutes, stopped heating slows down mixing velocity, and allows compositions cooling lentamente.In parafacies, add the deionized water of (compositions final total weight %'s) 15.5 % by weight, and add lentamente following composition and mix until hydration: the PVMMA copolymer ((
Figure BPA00001701982700641
S-97BF; ISP Corp., Wayne, NJ, USA) and sodium hydroxide (20% active component).Solution is with thickening slightly.In-process pH should be 6.90-7.00.Heat described parafacies to 50-55 ℃.Add lentamente under very strong mixing polyquaternary ammonium salt-28 (
Figure BPA00001701982700642
NT-20; ISPCorp.).Solution will become opaque and become low-viscosity.Cooling described parafacies, and add the DMDM Hydantoin of (compositions final total weight %'s) 0.05 % by weight under≤45 ℃.Lentamente parafacies is added into principal phase under≤45 ℃.Then add following composition:
Figure BPA00001701982700643
TQuat 60 (siloxane quaternary ammonium-22; Evonik, Essen, Germany), propylene glycol, the DMDM Hydantoin of flavouring agent and (compositions final total weight %'s) 0.15 % by weight.
For compositions 4C, add the deionized water of (compositions final total weight %'s) 52.45 % by weight in principal phase.Begin to be heated to 80-85 ℃.Once add following a kind of composition and mixing until dissolving and the solution clarification that becomes fully: EDETATE SODIUM and L-Aspartic acid.Add following a kind of composition next time and mix until melting at 80-85 ℃: SAPDMA (checking to guarantee that solution becomes clarification), spermol and glyceryl stearate.Mixed consumingly under 80-85 ℃ 30 minutes.After 30 minutes, stopped heating slows down mixing velocity, and allows compositions cooling lentamente.In parafacies, add the deionized water of (compositions final total weight %'s) 15.5 % by weight, and add lentamente following composition and mix until hydration: the PVMMA copolymer (
Figure BPA00001701982700651
S-97BF; ISP Corp., Wayne, NJ, USA) and sodium hydroxide (20% active component).Solution is with thickening slightly.In-process pH should be 6.90-7.00.Heat described parafacies to 50-55 ℃.Add lentamente under very strong mixing polyquaternary ammonium salt-28 (
Figure BPA00001701982700652
NT-20; ISP Corp.).Solution will become opaque and become low-viscosity.Cooling described parafacies, and add the DMDM Hydantoin of (compositions final total weight %'s) 0.05 % by weight under≤45 ℃.Lentamente parafacies is added into principal phase in the time of≤45 ℃.Premixing quaternary ammonium salt-80/ propylene glycol and polydimethylsiloxane also are added in the principal phase and parafacies of merging subsequently.Then add following composition: DC-8500 (two (C13-15 alkoxyl) PG-ammonia end polydimethylsiloxane, Dow Coming, Midland, MI, USA), propylene glycol, the DMDM Hydantoin of flavouring agent and (compositions final total weight %'s) 0.15 % by weight.
For compositions 4D, add the deionized water of (compositions final total weight %'s) 40 % by weight.Add lentamente following composition, and mixing is until hydration: the PVMMA copolymer (
Figure BPA00001701982700653
S-97BF (ISP)) and sodium hydroxide (20% active component).Solution is with thickening slightly.In-process pH should be 6.90-7.00.Be heated to 50-55 ℃, and add lentamente under very strong mixing polyquaternary ammonium salt-28 (
Figure BPA00001701982700654
NT-20; ISP Corp.).Solution will become opaque and become low-viscosity.Begin to be heated to 80-85 ℃, and once add following a kind of composition, mix until dissolving fully: the deionized water of EDETATE SODIUM, L-Aspartic acid and (compositions final total weight %'s) 22.95 % by weight.Add following a kind of composition next time and mix until melting at 80-85 ℃: SAPDMA, spermol, stearyl alcohol, glyceryl stearate, Crodamol STS (PPG-3 benzyl oxide myristinate; Croda, Inc., Edison, NJ, USA),
Figure BPA00001701982700655
SC 96 (65% polyquaternary ammonium salt-37,25% propylene glycol dicaprylate/dicaprate, 10%PPG-1 tridecyl alcohol polyethers-6;
Figure BPA00001701982700656
/ BASF, Basel, Switzerland).Mixed consumingly under 80-85 ℃ 30 minutes.Slow down mixing velocity and allow composition cools.When temperature≤45 ℃, add following composition: D5/D6/ polydimethylsiloxane, propylene glycol, flavouring agent and DMDM Hydantoin.
For compositions 4E, add the deionized water of (compositions final total weight %'s) 50.47 % by weight in principal phase.Begin to be heated to 80-85 ℃.Once add following a kind of composition and mixing until dissolving and the solution clarification that becomes fully: EDETATE SODIUM and L-Aspartic acid.Add following a kind of composition next time and mix until melting at 80-85 ℃: SAPDMA (checking to guarantee that solution becomes clarification), spermol, glyceryl stearate,
Figure BPA00001701982700661
202 (arachidic alcohol and behenyl alcohol and Semen arachidis hypogaeae base glucosides; SEPPIC, Paris, France), and the aminopropyl dimethione.Mixed consumingly under 80-85 ℃ 30 minutes.After 30 minutes, stopped heating slows down mixing velocity, and allows compositions cooling lentamente.In parafacies, add the deionized water of (compositions final total weight %'s) 15.5 % by weight, and add lentamente following composition and mix until hydration: the PVMMA copolymer (
Figure BPA00001701982700662
S-97 BF; ISP Corp., Wayne, NJ, USA) and sodium hydroxide (20% active component).Solution is with thickening slightly.In-process pH should be 6.90-7.00.Heat described parafacies to 50-55 ℃.Add lentamente under very strong mixing polyquaternary ammonium salt-28 (
Figure BPA00001701982700663
NT-20; ISP Corp.).Solution will become opaque and become low-viscosity.Cooling described parafacies, and add the DMDM Hydantoin of (compositions final total weight %'s) 0.05 % by weight under≤45 ℃.Lentamente parafacies is added into principal phase in the time of≤45 ℃.In the situation that 45 ℃ or lower the interpolation
Figure BPA00001701982700664
2001 (polyquaternary ammonium salt-47; Nalco, Naperville, IL, USA).Premixing D5/ dimethiconol and polydimethylsiloxane also are added in the principal phase and parafacies of merging subsequently.Then add following composition: DC-8500 (two (C13-15 alkoxyl) PG-ammonia end polydimethylsiloxane, Dow Coming, Midland, MI, USA), propylene glycol, the DMDM Hydantoin of flavouring agent and (compositions final total weight %'s) 0.15 % by weight.
Embodiment 6
The present embodiment has illustrated the reparation of the furcated end of hair fiber, and it uses method of testing of the present invention.
The compositions of hereinafter relatively using in this research, it is shown in Figure 1.If necessary, regulate to obtain suitable pH with sodium hydroxide/aspartic acid.
Compositions 6A-6D
Figure BPA00001701982700671
The compositions of hereinafter relatively using in this research, as shown in Figure 2.If necessary,
Figure BPA00001701982700681
Regulate to obtain suitable pH with sodium hydroxide/citric acid/aspartic acid.
Compositions 6E-6J
Figure BPA00001701982700691
Figure BPA00001701982700701
Fig. 1 has shown when European's hair of the furcated end with machine-building of using twice bleaching, the result that conditioner is repaired.This result has shown uses the washing-off type conditioner to obtain approximately 80% reparation in three circulations.
Fig. 2 has shown when European's hair of the furcated end with machine-building of using twice bleaching, the result of multiple combination thing.This result is based on all preparations and comprises this supposition of leave preparation of spending the night and repairing.This result has shown that all leave compositionss repair all greater than 80% in single treatment.
Embodiment 7
The present embodiment has illustrated the reparation of the furcated end of hair fiber, and it uses method of testing of the present invention.
The compositions of hereinafter relatively using in this research.If necessary, regulate to obtain suitable pH with sodium hydroxide/aspartic acid.
Compositions 7A-7D
Figure BPA00001701982700702
Figure BPA00001701982700711
Goal standard 7A:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 5,000-15,000 centipoise
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: opaque Emulsion
Goal standard 7B:
pH:5.5-6.5
Viscosity (LVT/ rotor 4/30rpm/1 minute, 25 ℃): 15,000-20,000 centipoise
Color: white/cream-coloured (MS)
Abnormal smells from the patient: MS
Outward appearance: viscosity, opaque Emulsion
Goal standard 7C:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 15,000-25,000 centipoise
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: viscosity, opaque Emulsion
Goal standard 7D:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 10,000-20,000 centipoise
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: opaque Emulsion
Remove 50 hair fibers that contain furcated end from topknot.Described hair fiber sample is placed on microscope slide, along a two-sided tape alignment that is used for optical imagery.Before product is used, use to have that transmission is photoemissive carries out independent imaging with the about WILD stereoscopic microscope of 25 * amplification to selected each fiber with furcated end, and memory image.Also described fiber is being rotated to guarantee that furcated end is within field range before picture catching.
Carry out according to hereinafter listed product application program.In each case, 50 selected fibers with furcated end are arranged as respectively in five different topknots, and products applied then.Again obtain the optical imagery of tip of each selected fiber to check and to assess the degree that furcated end is repaired.Result is shown in table 12.
Table 12 has shown the comparison process total quantity (50) and the processing summary of the furcated end data research of the quantity of the furcated end of reparation afterwards of furcated end before.(by independent method for the preparation of repeat research (classification 6) furcated end).
Table 12
Figure BPA00001701982700731
All classifications have all shown the ability of repairing the furcated end in hair fiber, and in them three kinds demonstrate 90% or larger improvement.
The product application program
Scheme is listed with the order shown in table 12.For some compositions (following pointed), in order to obtain 80% dried bundle, make the time of drying up become 20 minutes by the characteristic (gentle air flow) of hair-dryer from 5 minutes.
A, prerinse hair
1, by cleaning the hair that becomes silvery white (2X) with the bleaching of wax combination in Sodium Lauryl Ether Sulphate (1M) solution that is immersed in 5%w/w.Solution is 40: 1 than hair.At room temperature soak 30 minutes, and then with hands massage hair 3 minutes, afterwards with the tap water rinsing of 40 ℃ until all foams are all rinsed out.
2, utilize thin paper or towel to blot hair, comb is straight, and makes described hair dried overnight under ambient room temperature.
B, machinery produce furcated end
1, this bundle is taken a sample take the density of hair as linear mode by international hair importer (Internation Hair Importers).Preparing 5 width is 1.5 " topknot, cut and tie up and make each topknot have the hair of 6g.
2, each topknot is attached to carding machine repeatedly, and every side combing topknot 1500 times, each topknot is 3000 combings altogether.
3, in carding process, hair-dryer is placed in topknot and sets at a distance of position and the high heat of unlatching of 8 inches.Make hair be pushed to comb in the process of recarding air flow the lead bottom of topknot.
C, select furcated end and gather initial pictures from topknot
1, use magnifier, check that the end of topknot is to find the hair fiber with furcated end.Select and connect root to remove 50 fibers with furcated end from described topknot.Select 10 furcation area end fibers from each topknot, make and to transfer to 50 fibers from five topknots.
2, use metal to be crimped onto the curling described fiber of tip, curling arranged in columns the making that then will be arranged on band has 10 fibers on each adhesive tape.Using another adhesive tape to cover describedly curlingly makes them to be mentioned together easily.
3, give 50 all fiber numberings, and gather the optical imagery of 10 in 50 hair fibers, be used for before and contrast photo afterwards.
4, use red permanent marker, with each labelling in selected 50 fibers until bifurcated initial.
5, by furcated end being arranged on the optical imagery that gathers 10 furcation area ends on microscope slide.Use stereoscopic microscope from microscopical dressing table below transmission light with 50 * the amplification images acquired.
6, check other 40 fibers with furcated end with described stereoscopic microscope, but they do not need to take a picture.
7, the article tape that contains furcated end is placed on 1.5 " centre of topknot.
8, use large clip, for example binder clamps the topknot with furcated end fiber.
D, compositions are used-classification 1
1, in the water of 35-40 ℃ with 1GPM moistening topknot 30 seconds.
2, the shampoo with the non-conditioning of 1.5ml is applied to 1.5 inches topknots and massaged 1 minute.
3, in the water of 35-40 ℃ with 1GPM rinsing topknot 30 seconds.
4, come lemon to fall excessive water by slip topknot between referring to.
5, the top with topknot is mounted to be used to the stand that dries up.
6, utilize hair clip at 3/4 length place of topknot, it to be clamped to avoid the hair migration.
7, use the drying machine away from 2 feet of topknots to dry up described topknot approximately 3 minutes with middle heat.
8, the compositions 7A (leave inorganic agent) with 1.5ml evenly is applied on the both sides of 1.5 feet moist topknots.Mainly endways and be easy to occur furcated end zone massage 1 minute.
9, in every side combing of topknot once.
10, the top with topknot is mounted to be used to the stand that dries up.
11, at 3/4 length place of topknot, it is clamped to avoid the hair migration with hair clip.
12, use away from the drying machine of 2 feet of topknots take middle heat (gentle air flow) dry up described topknot approximately 20 minutes until it is as 80% drying.
13, dry up after, the combing topknot is once on every side.
D, compositions are used-classification 2
1, in the water of 35-40 ℃ with 1GPM moistening topknot 30 seconds.
2, the compositions 7B (shampoo) with 1.5ml is applied to 1.5 inches topknots and massaged 1 minute.
3, rinsed topknot 30 seconds with 1GPM in the water of 35-40 ℃.
4, twist off excessive water by slip topknot between referring to.
5, the compositions 7C (conditioner) with 1.5ml is applied to 1.5 inches topknots, and knocks topknot 9 times from the top to the bottom, and makes its standing 1 minute.
6, in the water of 35-40 ℃ with 1GPM rinsing topknot 30 seconds.
7, use Kim Wipes leniently to blot topknot.
8, the top with topknot is mounted to be used to the stand that dries up.
9, utilize hair clip at 3/4 length place of topknot, it to be clamped to avoid the hair migration.
10, use away from the drying machine of 2 feet of topknots and did described topknot approximately 3 minutes with middle hot blow.
11, the compositions 7A (leave inorganic agent) with 1.5ml is applied on 1.5 feet moist topknots.Mainly endways and be easy to occur furcated end zone massage 1 minute.
12, in every side combing of topknot once.
13, the top with topknot is mounted to be used to the stand that dries up.
14, utilize hair clip at 3/4 length place of topknot, it to be clamped to avoid the hair migration.
15, use away from the drying machine of 2 feet of topknots take middle heat (gentle air flow) dry up described topknot approximately 20 minutes until it is as 80% drying.
16, dry up after, the combing topknot is twice on every side.
D, compositions are used-classification 3
1, in the water of 35-40 ℃ with 1GPM moistening topknot 30 seconds.
2, the shampoo with the non-conditioning of 1.5ml is applied to 1.5 inches topknots and massaged 1 minute.
3, in the water of 35-40 ℃ with 1GPM rinsing topknot 30 seconds.
4, twist off excessive water by slip topknot between referring to.
5, the top with topknot is mounted to be used to the stand that dries up.
6, utilize hair clip at 3/4 length place of topknot, it to be clamped to avoid the hair migration.
7, use away from the drying machine of 2 feet of topknots and did described topknot approximately 3 minutes with middle hot blow.
8, the compositions 7D (inorganic agent spends the night) with 1.5ml is applied on the both sides of 1.5 feet moist topknots.Mainly endways and be easy to occur furcated end zone massage 1 minute.
9, in every side combing of topknot once.
10, because this is processings of spending the night, so that compositions remains on hair upper 8 hour.
11, utilize hair clip at 3/4 length place of topknot, it to be clamped to avoid the hair migration.
D, compositions are used-classification 4
1, in the water of 35-40 ℃ with 1GPM moistening topknot 30 seconds.
2, the shampoo with the non-conditioning of 1.5ml is applied to 1.5 inches topknots and massaged 1 minute.
3, in the water of 35-40 ℃ with 1GPM rinsing topknot 30 seconds.
4, twist off excessive water by slip topknot between referring to.
5, the compositions 7C with 1.5ml is applied to 1.5 inches topknots, and knocks topknot 9 times from the top to the bottom, and makes its standing 1 minute.
6, in the water of 35-40 ℃ with 1GPM rinsing topknot 30 seconds.
7, use Kim Wipes leniently to blot topknot.
8, the top with topknot is mounted to be used to the stand that dries up.
9, utilize hair clip at 3/4 length place of topknot, it to be clamped to avoid the hair migration.
10, use away from the drying machine of 2 feet of topknots take middle hot blow do described topknot approximately 5 minutes until it is as 80% drying.
11, twice of combing topknot on every side.
12, again apply red-label after drying up on fiber.
13,2 extra circulations of repeating step 1-12 are again processed thereby altogether carry out three times.
D, compositions are used-classification 5
1, in the water of 35-40 ℃ with 1GPM moistening topknot 30 seconds.
2, the compositions 7B (shampoo) with 1.5ml is applied to 1.5 inches topknots and massaged 1 minute.
3, in the water of 35-40 ℃ with 1GPM rinsing topknot 30 seconds.
4, wring out excessive water by slip topknot between referring to.
5, the compositions 7C (conditioner) with 1.5ml is applied to 1.5 inches topknots, and knocks topknot 9 times from the top to the bottom, and makes its standing 1 minute.
6, in the water of 35-40 ℃ with 1GPM rinsing topknot 30 seconds.
7, use Kim Wipes leniently to blot topknot.
8, the combing topknot is once on every side.
9, the top with topknot is mounted to be used to drying up stand.
10, utilize hair clip at 3/4 length place of topknot, it to be clamped to avoid the hair migration.
11, use away from the drying machine of 2 feet of topknots take middle heat (gentle air flow) dry up described topknot approximately 20 minutes until it is as 80% drying.
12, twice of combing on every side.
13, two extra circulations of repeating step 1-12 again, thereby total coprocessing three times.
E, select furcated end and gather final image from topknot
1, from 1.5 " centre of topknot removes the band that contains furcated end.
2, use stereoscopic microscope, by furcated end is arranged on microscope slide, gather optical imagery after the processing of 10 hair fibers with furcated end.
3, use other 40 fibers with furcated end of stereomicroscopy.
Thereby 4, count the fiber number that has been repaired and determine to repair %.
Embodiment 8
The present embodiment has illustrated the method that furcated end reparation situation is conveyed to consumer.
Fig. 3 uses compound polyelectrolyte (PEC) to repair the schematic diagram of furcated end for showing.Shown the possible mechanism of action of PEC here, wherein they are attached to the position of furcated end, self form network and assemble with fiber, and shrinking along with their dryings, and furcated end thus internally bonds.
Fig. 4 A-4D has shown and has repaired the still image of various types of furcated end with method described herein with compositions described herein.
Fig. 5 has shown from repair the tableaux of the video of furcated end by the technique of restorative procedure described herein.
Embodiment 9
The present embodiment has illustrated other compositions of the present invention.
Compositions 9A
Figure BPA00001701982700781
Figure BPA00001701982700791
Figure BPA00001701982700801
Goal standard 9A:
pH:6.0-7.0
Viscosity (RV T-C, 5rpm, 1 minute, 25 ℃): 40,000-80,000
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque (muddy) gel
Compositions 9B-1 and 9B-2
Figure BPA00001701982700802
Figure BPA00001701982700811
Goal standard 9B:
Figure BPA00001701982700812
Figure BPA00001701982700821
Compositions 9C-1
Figure BPA00001701982700822
Figure BPA00001701982700831
Goal standard 9C-1:
pH:4.0-5.0
Color: muddy/pale
Abnormal smells from the patient: match reference
Outward appearance: Lac Bovis seu Bubali shape liquid
Compositions 9C-2
Figure BPA00001701982700832
Figure BPA00001701982700841
Goal standard 9C:
pH:4.5-6
Color: white
Abnormal smells from the patient: match reference
Outward appearance: Lac Bovis seu Bubali shape liquid
Compositions 9D-1 and 9D-2
Figure BPA00001701982700851
Goal standard 9D:
Body
Color: cream-coloured (MS)
Abnormal smells from the patient: MS
Outward appearance: troubled liquor
pH:5.0-6.5
Proportion: *0.986
Involatile constituent: 4.4-4.9%
(T=4.66)
Finished product
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: dense foam, non-water sample, do not trickle
pH:5.0-6.5
Foam stability: 200 seconds minutes
Foam density: *0.039g/mL
Proportion: *0.941
4.3-4.8%
Involatile constituent: (T=4.58)
*Be used for reference
Compositions 9E
Figure BPA00001701982700862
Figure BPA00001701982700871
Figure BPA00001701982700881
Goal standard 9E:
pH:6.0-7.0
Viscosity (RV T-C, 5rpm, 1 minute, 25 ℃): 40,000-80,000
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque (muddy) gel
Compositions 9F-1 to 9F-4
Figure BPA00001701982700891
Figure BPA00001701982700901
Goal standard 9F:
pH:7.00-7.50
Viscosity (RV T-C, 5rpm, 1 minute, 25 ℃): 50,000-100,000cps
Color: transparent-mute white
Abnormal smells from the patient: MS
Outward appearance: thick gel
Compositions 9G-1 to 9G-4
Figure BPA00001701982700902
Figure BPA00001701982700911
Goal standard 9G:
pH:5.00-6.50
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 20,000-40,000cps
Color: translucent white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque gel
Compositions 9H-1 to 9H-2
Figure BPA00001701982700921
Figure BPA00001701982700931
Goal standard 9H:
pH:5.00-6.50
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 5,000-15,000cps
Color: translucent white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, Lac Bovis seu Bubali shape liquid
Compositions 9I-1 to 9I-3
Figure BPA00001701982700951
Goal standard 9I:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 20,000-30,000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque emulsion
Compositions 9J-1 to 9J-3
Figure BPA00001701982700952
Figure BPA00001701982700961
Goal standard 9J:
pH:7.0-8.0
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 5,000-15,000cps
Color: colourless-faint yellow
Abnormal smells from the patient: MS
Outward appearance: the oil-based liquid of slight haze
Compositions 9K-1 to 9K-3
Figure BPA00001701982700971
Goal standard 9K:
pH:7.0-8.0
Viscosity (RV T-C, 10rpm, 1 minute, 25 ℃): 50,000-100,000cps
Color: transparent-mute white
Abnormal smells from the patient: MS
Outward appearance: thick gel-dilute liquid
Compositions 9L
Figure BPA00001701982700991
Goal standard 9L:
pH:3.20-4.50
Infiltration (50g weight w/ cone): 18-24mm
Color: colourless
Abnormal smells from the patient: MS
Outward appearance: thick gel
Compositions 9M
Composition % by weight
Principal phase
Deionized water 31.2837
Gantrez AN-119 (Gantrez S-97BF (ISP)) 0.001
Sodium hydroxide, 20% 0.00125
Add following component and mix consumingly
Polyquaternary ammonium salt-28 (Conditioneze NT-20 (ISP), 20% active component) 0.045
Add lentamente following component, mix until hydration
Polyquaternary ammonium salt 10 0.8
Being heated to 50 ℃ also mixes until clarification
EDETATE SODIUM 0.1
Cocamido propyl betaine (approximately 30% active component), water, sodium chloride 8.2
NaOH,20% 0.14875
Sodium laureth sulfate-1 mole (25%) 32
Laureth disodium sulfosuccinate (approximately 34% active component) 12.8
Styrene/VP copolymer (40%), water 0.75
PEG-6 caprylic/capric triglyceride 0.6
Kathon CG 0.07
Flavouring agent 0.7
Cocoa Cortex cocois radicis (Cortex cocois radicis) oil 0.0001
Keratin aminoacid 0.0001
Flower/leaf extract 0.0001
The component that premixing is following also is added into batch of material
Deionized water 10
Sodium chloride 2.5
Goal standard 9M:
pH:5.5-6.5
Viscosity (LVT/ rotor 4/30rpm/1 minute, 25 ℃): 15,000-20,000cps
Color: white/cream-coloured (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque liquid
Compositions 9N-1 and 9N-2
Figure BPA00001701982701011
Figure BPA00001701982701021
Figure BPA00001701982701031
Goal standard 9N:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 15,000-25,000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque emulsions
Compositions 9O
Figure BPA00001701982701032
Figure BPA00001701982701041
Goal standard 9O:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 5,000-15,000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: opaque emulsion
Compositions 9P
Figure BPA00001701982701051
Figure BPA00001701982701061
Goal standard 9P:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃): 10,000-20,000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: opaque emulsions
Compositions 9Q
Composition % by weight
Principal phase
Deionized water 52.8
EDETATE SODIUM 0.05
L-Aspartic acid 0.75
Under 80-85 ℃ each add following a kind of, and mixing until melting/evenly
SAPDMA 2
Spermol 1
Glyceryl stearate 0.2
The aminopropyl dimethione 0.5
Mixed consumingly under 80-85 ℃ 30 minutes
Slow down mixing velocity and allow cooling
Parafacies
Deionized water 15.5
Add lentamente following component, mix until hydration
Gantrez AN-119 (Gantrez S-97BF (ISP)) 0.2
Sodium hydroxide (20% active component) 0.25
(solution is with thickening slightly)
In-process pH regulation: 6.90-7.00
The heating parafacies is to 50-55 ℃
Add lentamente following component under very strong mixing
Polyquaternary ammonium salt-28 (Conditioneze NT-20 (ISP), 20% active component) 9
(solution will become opaque and the viscosity step-down)
Add following component under≤45 ℃
DMDM Hydantoin 0.05
Lentamente parafacies is added into principal phase under≤45 ℃
<45℃
Ensuing two of premixing
DS, polydimethylsiloxane 2
Polydimethylsiloxane (60,000cst) 1
DC-8500 1
Propylene glycol 10
Flavouring agent 0.5
DMDM Hydantoin 0.2
Salcare SC-96 3
Goal standard 9Q:
pH:4.50-6.00
Viscosity (RV T-8,10rpm, 1 minute, 25 ℃):
Bulk viscosity: 7,000-15,0000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: opaque emulsions
Compositions 9R
Composition % by weight
Principal phase
Deionized water 40.55
Add lentamente following component, mix until hydration
Gantrez AN-119 (Gantrez S-97BF (ISP)) 0.2
Sodium hydroxide (20% active component) 0.25
(solution is with thickening slightly)
In-process pH regulation: 6.90-7.00
Be heated to 50-55 ℃
Add lentamente following component under very strong mixing
Polyquaternary ammonium salt-28 (Conditioneze NT-20 (ISP), 20% active component) 9
(solution will become opaque and the viscosity step-down)
Begin to be heated to 80-85 ℃
The following a kind of component of each interpolation is mixed until dissolving fully
EDETATE SODIUM 0.05
L-Aspartic acid 0.75
Deionized water 20.27
Add following a kind of component and mix until melting at every turn under 80-85 ℃/evenly
SAPDMA 2
Spermol 4
″Montanov 202″ 1.18
Glyceryl stearate 0.80
" Crodamol STS " (myristic acid benzyl oxide) 2
Salcare SC-96 1
The aminopropyl dimethione 0.75
Mixed consumingly under 80-85 ℃ 30 minutes
Slow down mixing velocity and allow cooling
<45℃
Ensuing two of premixing
DS, polydimethylsiloxane 3
Polydimethylsiloxane 1.5
DC 2-8566 (ammonia end polydimethylsiloxane) 2
Propylene glycol 10
Flavouring agent 0.5
DMDM Hydantoin 0.2
Goal standard 9R:
pH:4.50-6.00
Viscosity (RV T-8,10rpm, 1 minute,
25℃):
Bulk viscosity: 15,000-25,000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: opaque emulsion
Compositions 9S-1 to 9S-6
Figure BPA00001701982701091
Figure BPA00001701982701101
Figure BPA00001701982701111
Goal standard 9S (also for compositions 6J):
Compositions 9T
Composition % by weight
Principal phase
Deionized water 40.55
Add lentamente following component, mix until hydration
Gantrez AN-119 (Gantrez S-97BF (ISP)) 0.2
Sodium hydroxide (20% active component) 0.25
(solution is with thickening slightly)
In-process pH regulation: 6.90-7.00
Record pH:6.95
Be heated to 50-55 ℃
Add lentamente following component under very strong mixing
Polyquaternary ammonium salt-28 (Conditioneze NT-20 (ISP)) 9
(solution will become opaque and the viscosity step-down)
Deionized water 39.05
EDETATE SODIUM 0.05
Salcare SC-96 3
Mix until evenly
<45℃
Polydimethylsiloxane (DC-200,20cst) 3
Phenyl trimethyl polysiloxanes (DC-556) 2
Cyclopentasiloxane, polydimethylsiloxane 1
Glycerol 1
Propylene glycol 0.5
Flavouring agent 0.2
DMDM Hydantoin 0.2
Goal standard 9T:
pH:5.00-6.50
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃)
Bulk viscosity: 7,000-15,000cps
Color: translucent white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, Lac Bovis seu Bubali shape fluid
Compositions 9U
Composition % by weight
Principal phase
Deionized water 60.85
EDETATE SODIUM 0.05
L-Aspartic acid 0.75
Add following a kind of component and mix until melting at every turn under 80-85 ℃/evenly
SAPDMA 2
Spermol 1
Tristerin 0.2
Mixed consumingly under 80-85 ℃ 30 minutes
Slow down mixing velocity; Allow cooling and reduce foam
Parafacies
Deionized water 15.50
Add lentamente following component; Mix until hydration
Gantrez AN-119 (Gantrez S-97BF (ISP)) 0.2
Sodium hydroxide (20% active component) 0.25
(solution is with thickening slightly)
In-process pH regulation: 6.90-7.00
The heating parafacies is to 50-55 ℃
Add lentamente following component under very strong mixing
Polyquaternary ammonium salt-28 (Conditioneze NT-20 (ISP)) 9
(solution will become opaque and the viscosity step-down)
(mixing~10 minutes)
Add following component under≤45 ℃
DMDM Hydantoin 0.05
Lentamente parafacies is added into principal phase under≤45 ℃
<45℃
The siloxanes premix
Polydimethylsiloxane (60,000cst) 2
Phenyl gathers trimethicone (DC-556) 2
DS, polydimethylsiloxane (DC-1501) 1
Glycerol 1
Propylene glycol 0.5
Flavouring agent 0.5
DMDM Hydantoin 0.15
Salcare SC-96 3
Goal standard 9U:
pH:4.5-6.50
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃)
Bulk viscosity: 8,000-16,000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: opaque emulsions
Compositions 9V-1 to 9V-3
Figure BPA00001701982701141
Figure BPA00001701982701151
Goal standard 9V:
pH:6.5-7.5
Viscosity (RV T-C, 5rpm, 1 minute, 25 ℃):
Volume: 40,000-90,000
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque gel
Compositions 9W-1 to 9W-3
Figure BPA00001701982701162
Figure BPA00001701982701171
Figure BPA00001701982701181
Goal standard 9W:
pH:4.5-6.00
Viscosity (RV T-8,10rpm, 1 minute, 25 ℃): 15,000-25,000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque emulsions
Compositions 9X-1 and 9X-2
Figure BPA00001701982701182
Goal standard 9X:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1 minute, 25 ℃):
Bulk viscosity: 7,000-15,000cps
W/ shear viscosity (finished product): 20,000-35,000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque emulsions
Embodiment 10
The present embodiment has illustrated exemplary interpolation speed, interpolation time, temperature, mixing velocity and the incorporation time for the preparation of PEC.
-water density: Perry ' s Chemical Engineer ' s Handbook.
-NaOH 20% density=1.2191kg/L and Conditioneze density=1.042kg/L.
A 270-kg batch of material
The PEC complex is in only having 113 liters/30 gallons premixing containers of center turbine stirrer
Main batch of material is in having center turbine and side and sweeping 227 liters/60 gallons mixers of agitator
The machined parameters of PEC complex:
The initial water loadings=42.02L (41.85kg)
Add speed=28L/min (28kg/min)
Total interpolation time=1.5min
Initial water temperature=29 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Gantrez AN-119(Gantrez S-97BF)=0.54kg (solid)
Add speed=0.6kg/min
Total interpolation time=1min
Temperature=30 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Disperse incorporation time=30min
Sodium hydroxide, 20%=0.55L (0.675kg)
Add speed=0.6L/min (0.7kg/min)
Total interpolation time=1min
Temperature=30 ℃
Center turbine stirrer=slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Hydration incorporation time=20min
In-process pH checks=6.90
Heating pre-composition 10 minutes to 51 ℃
Polyquaternary ammonium salt 28 (Conditioneze NT-20)=23.32L (24.30kg)
Add speed=3.33L/min (3.47kg/min)
Total interpolation time=7min
Temperature=49 ℃
(RPM) of center turbine stirrer=moderate/strong clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Compound incorporation time=40min
Premix is cooling
Be cooled to 29 ℃
Center turbine stirrer=very slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Cooling and mixing time=60min *
( *Annotate: incorporation time has reflected makes main batch of material reach the PEC premix interpolation required time of point)
One 11, the 800-kg batch of material
The PEC complex is in having center turbine and side and sweeping 5,678 liters/1,500 gallon premixing container of agitator
Main batch of material has center turbine and side and is sweeping the M0112 of agitator, in 113 liters/3,200 gallons mixers
The machined parameters of PEC complex:
The initial water loadings=1840.9L (1835kg)
Add speed=526L/min (524kg/min)
Total interpolation time=3.5min
Temperature=26 ℃
Center turbine stirrer=25RPM counterclockwise
Side is swept agitator=7RPM clockwise
Gantrez AN-119(Gantrez S-97BF)=23.6kg (solid)
Add speed=7.87kg/min
Total interpolation time=3min
Temperature=27 ℃
Center turbine stirrer=20RPM counterclockwise
Side is swept agitator=7RPM clockwise
Disperse incorporation time=30min
Sodium hydroxide, 20%=24.2L (29.5kg)
Add speed=12.1L/min (14.75kg/min)
Total interpolation time=2min
Temperature=27 ℃
Center turbine stirrer=20RPM counterclockwise
Side is swept agitator=7RPM clockwise
Hydration incorporation time=10min
In-process pH checks=6.72.Add NaOH and the pH=6.80 of 118 extra grams (0.001 % by weight).Add NaOH and the pH=6.90 of 118 extra grams (0.001 % by weight).The NaOH of 29.736kg altogether
Heating pre-composition 18 minutes to 55 ℃
Polyquaternary ammonium salt 28 (Conditioneze NT-20)=1019L (1062kg)
Add speed=29.1L/min (30.0kg/min)
Total interpolation time=35min
Temperature=54 ℃
Center turbine stirrer=28RPM counterclockwise
Side is swept agitator=7RPM clockwise
Compound incorporation time=30min
Premix is cooling
Be cooled to 35 ℃
Center turbine stirrer=18RPM counterclockwise
Side is swept agitator=7RPM clockwise
Cooling and mixing time=240min *
( *Annotate: incorporation time has reflected makes main batch of material reach the PEC premix interpolation required time of point)
A 270-kg batch of material
The PEC complex is in only having 113 liters/30 gallons premixing containers of center turbine stirrer
Main batch of material is in having center turbine and side and sweeping 227 liters/60 gallons mixers of agitator
The machined parameters of PEC complex:
The initial water loadings=42.04L (41.84kg)
Add speed=28L/min (28kg/min)
Total interpolation time=1.5min
Initial water temperature=31 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) mixer
Heating pre-composition 10 minutes to 52 ℃
Gantrez AN-119(Gantrez S-97BF)=0.54kg (solid)
Add speed=0.6kg/min
Total interpolation time=1min
Temperature=52 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Disperse incorporation time=25min
Sodium hydroxide, 20%=0.56L (0.688kg)
Add speed=0.6L/min (0.7kg/min)
Total interpolation time=1min
Temperature=52 ℃
Center turbine stirrer=slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Hydration incorporation time=15min
In-process pH checks=6.93
Polyquaternary ammonium salt 28 (Conditioneze NT-20)=23.32L (24.30kg)
Add speed=4.66L/min (4.86kg/min)
Total interpolation time=5min
Temperature=53 ℃
(RPM) of center turbine stirrer=moderate/strong clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Compound incorporation time=40min
Premix is cooling
Be cooled to 29 ℃
Center turbine stirrer=very slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Cooling and mixing time=100min *
( *Annotate: incorporation time has reflected makes main batch of material reach the PEC premix interpolation required time of point)
A 270-kg batch of material
The PEC complex is in only having 113 liters/30 gallons premixing containers of center turbine stirrer
Main batch of material is in having center turbine and side and sweeping 227 liters/60 gallons mixers of agitator
PEC complex machined parameters:
The initial water loadings=42.03L (41.85kg)
Add speed=28L/min (28kg/min)
Total interpolation time=1.5min
Initial water temperature=30 ℃
The center turbine stirrer=appropriateness (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Gantrez AN-119(Gantrez S-97BF)=0.54kg (solid)
Add speed=0.6kg/min
Total interpolation time=1min
Temperature=30 ℃
The center turbine stirrer=appropriateness (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Disperse incorporation time=30min
Sodium hydroxide, 20%=0.56L (0.68kg)
Add speed=0.6L/min (0.7kg/min)
Total interpolation time=1min
Temperature=31 ℃
Center turbine stirrer=slow (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Hydration incorporation time=6min
In-process pH inspection=initial 6.83.Add NaOH and the pH=6.95 of 2.7 extra grams (0.001 % by weight).The NaOH of 682.7g altogether
Heating pre-composition 10 minutes to 57 ℃
Polyquaternary ammonium salt 28 (Conditioneze NT-20)=23.32L (24.30kg)
Add speed=3.33L/min (3.47kg/min)
Total interpolation time=7min
Temperature=56 ℃
(RPM) of center turbine stirrer=moderate/strong clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Compound incorporation time=30min
Premix is cooling
Be cooled to 27 ℃
Center turbine stirrer=very slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Cooling and mixing time=120min *
( *Annotate: incorporation time has reflected makes main batch of material reach the PEC premix interpolation required time of point)
One 1, the 250-kg batch of material
The PEC complex is in having center turbine and side and sweeping 379 liters/100 gallons premixing containers of agitator
Main batch of material is in having center turbine and side and sweeping 1,893 liter/500 gallons mixers of agitator
The machined parameters of PEC complex:
The initial water loadings=195.2L (194.4kg)
Add speed=97.6L/min (97.2kg/min)
Total interpolation time=2min
Initial water temperature=29 ℃
Center turbine stirrer=60RPM counterclockwise
Side is swept agitator=10RPM clockwise
Gantrez AN-119(Gantrez S-97BF)=2.5kg (solid)
Add speed=1.3kg/min
Total interpolation time=2min
Temperature=31 ℃
Center turbine stirrer=60RPM counterclockwise
Side is swept agitator=10RPM clockwise
Disperse incorporation time=26min
Sodium hydroxide, 20%=2.56L (3.125kg)
Add speed=3L/min (4kg/min)
Total interpolation time=1min
Temperature=33 ℃
Center turbine stirrer=20RPM counterclockwise
Side is swept agitator=10RPM clockwise
Hydration incorporation time=11min
In-process pH checks=6.90
Heating pre-composition 10 minutes to 52 ℃
Polyquaternary ammonium salt 28 (Conditioneze NT-20)=108.0L (112.5kg)
Add speed=9.0L/min (9.4kg/min)
Total interpolation time=12min
Temperature=54 ℃
Center turbine stirrer=58RPM counterclockwise
Side is swept agitator=15RPM clockwise
Compound incorporation time=31min
Premix is cooling
Be cooled to 35 ℃
Center turbine stirrer=18RPM counterclockwise
Side is swept agitator=8RPM clockwise
Cooling and mixing time=135min *
( *Annotate: incorporation time has reflected makes main batch of material reach the PEC premix interpolation required time of point)
A 270-kg batch of material
The PEC complex is in only having 113 liters/30 gallons premixing containers of center turbine stirrer
Main batch of material is in having center turbine and side and sweeping 227 liters/60 gallons mixers of agitator
The machined parameters of PEC complex:
The initial water loadings=42.01L (41.84kg)
Add speed=28L/min (28kg/min)
Total interpolation time=1.5min
Initial water temperature=29 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Heating pre-composition 10 minutes to 52 ℃
Gantrez AN-119(Gantrez S-97BF)=0.54kg (solid)
Add speed=0.6kg/min
Total interpolation time=1min
Temperature=52 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Disperse incorporation time=25min
Sodium hydroxide, 20%=0.57L (0.69kg)
Add speed=0.6L/min (0.7kg/min)
Total interpolation time=1min
Temperature=53 ℃
Center turbine stirrer=slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Hydration incorporation time=5min
In processing, pH checks=6.95
Polyquaternary ammonium salt 28 (Conditioneze NT-20)=23.32L (24.30kg)
Add speed=4.66L/min (4.86kg/min)
Total interpolation time=5min
Temperature=53 ℃
(RPM) of center turbine stirrer=moderate/strong clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Compound incorporation time=35min
Premix is cooling
Be cooled to 30 ℃
Center turbine stirrer=very slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Cooling and mixing time=90min *
( *Annotate: incorporation time has reflected makes main batch of material reach the PEC premix interpolation required time of point)
A 270-kg batch of material
The PEC complex is in only having 113 liters/30 gallons premixing containers of center turbine stirrer
Main batch of material is in having center turbine and side and sweeping 227 liters/60 gallons mixers of agitator
The machined parameters of PEC complex:
The initial water loadings=42.01L (41.84kg)
Add speed=28L/min (28kg/min)
Total interpolation time=1.5min
Initial water temperature=29 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Gantrez AN-119(Gantrez S-97BF)=0.54kg (solid)
Add speed=0.6kg/min
Total interpolation time=1min
Temperature=30 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Disperse incorporation time=30min
Sodium hydroxide, 20%=0.56L (0.68kg)
Add speed=0.6L/min (0.7kg/min)
Total interpolation time=1min
Temperature=30 ℃
Center turbine stirrer=slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Hydration incorporation time=20min
In-process pH inspection=initial 6.81.Add NaOH and the pH=6.92 of 3.4 extra grams (0.00126 % by weight).The NaOH of 683.4g altogether
Heating pre-composition 10 minutes to 54 ℃
Polyquaternary ammonium salt 28 (Conditioneze NT-20)=23.32L (24.30kg)
Add speed=3.33L/min (3.47kg/min)
Total interpolation time=7min
Temperature=54 ℃
The clockwise direction of center turbine stirrer=moderate/strong (RPM)
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Compound incorporation time=35min
Premix is cooling
Be cooled to 35 ℃
Center turbine stirrer=very slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Cooling and mixing time=260min *
( *Annotate: incorporation time has reflected makes main batch of material reach the PEC premix interpolation required time of point)
One 3, the 772-kg batch of material
The PEC complex is in having center turbine and side and sweeping 1,893 liter/500 gallons premixing containers of agitator
Main batch of material is in having center turbine and side and sweeping 3,785 liters/1000 gallons mixers of agitator
The machined parameters of PEC complex:
The initial water loadings=588.93L (586.546kg)
Add speed=392.6L/min (391kg/min)
Total interpolation time=1.5min
Initial water temperature=29 ℃
Center turbine stirrer=46RPM counterclockwise
Side is swept agitator=10RPM clockwise
Gantrez AN-119(Gantrez S-97BF)=7.544kg (solid)
Add speed=3.77kg/min
Total interpolation time=2min
Temperature=29 ℃
Center turbine stirrer=46RPM counterclockwise
Side is swept agitator=10RPM clockwise
Disperse incorporation time=60min
Sodium hydroxide, 20%=7.735L (9.430kg)
Add speed=3.9L/min (4.7kg/min)
Total interpolation time=2min
Temperature=30 ℃
Center turbine stirrer=25RPM counterclockwise
Side is swept agitator=10RPM clockwise
Hydration incorporation time=10min
In-process pH checks=6.91
Heating pre-composition 10 minutes to 52 ℃
Polyquaternary ammonium salt 28 (Conditioneze NT-20)=325.80L (339.48kg)
Add speed=16.3L/min (17.0kg/min)
Total interpolation time=20min
Temperature=50 ℃
Center turbine stirrer=35RPM counterclockwise
Side is swept agitator=6RPM clockwise
Compound incorporation time=40min
Premix is cooling
Be cooled to 40 ℃
Center turbine stirrer=14RPM counterclockwise
Side is swept agitator=6RPM clockwise
Cooling and mixing time=55min *
( *Annotate: incorporation time has reflected makes main batch of material reach the PEC premix interpolation required time of point)
A 270-kg batch of material
The PEC complex is in only having 113 liters/30 gallons premixing containers of center turbine stirrer
Main batch of material is in having center turbine and side and sweeping 227 liters/60 gallons mixers of agitator
The machined parameters of PEC complex:
The initial water loadings=42.01L (41.84kg)
Add speed=28L/min (28kg/min)
Total interpolation time=1.5min
Initial water temperature=29 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Heating pre-composition 10 minutes to 52 ℃
Gantrez AN-119(Gantrez S-97BF)=0.54kg (solid)
Add speed=0.6kg/min
Total interpolation time=1min
Temperature=52 ℃
(RPM) of center turbine stirrer=moderate clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Disperse incorporation time=20min
Sodium hydroxide, 20%=0.57L (0.69kg)
Add speed=0.6L/min (0.7kg/min)
Total interpolation time=1min
Temperature=53 ℃
Center turbine stirrer=slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Hydration incorporation time=6min
In-process pH checks=6.98
Polyquaternary ammonium salt 28 (Conditioneze NT-20)=23.32L (24.30kg)
Add speed=4.66L/min (4.86kg/min)
Total interpolation time=5min
Temperature=53 ℃
(RPM) of center turbine stirrer=moderate/strong clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Compound incorporation time=35min
Premix is cooling
Be cooled to 29 ℃
Center turbine stirrer=very slowly (RPM) clockwise
Side is swept agitator=be not included in pilot scale (pilot) premixing container
Cooling and mixing time=100min *
( *Annotate: incorporation time has reflected makes main batch of material reach the PEC premix interpolation required time of point)
Embodiment 11
The present embodiment has been described the exemplary compositions (compositions 11A-11G) of the present invention.
The hair of some in these compositionss is repaired effect (together with compositions 1C) and is summarised in table 13 and 14.The curling conservation rate of the high humility of some in these compositionss is shown in Figure 7.
Compositions 11A
Figure BPA00001701982701351
Figure BPA00001701982701361
Goal standard 11A:
pH:5.00-6.50
Viscosity (RV T-B, 10rpm, 1min, 25 ℃): 20,000-40,000cps
Color: mute white (MS)
Abnormal smells from the patient: MS
Outward appearance: gel thickness, opaque
Compositions 11B
Figure BPA00001701982701362
Figure BPA00001701982701371
Goal standard 11B:
pH:6.0-7.5
Viscosity (RV T-C, 5rpm, 1min, 25 ℃): 50,000-100,000cps
Color: mute white
Abnormal smells from the patient: MS
Outward appearance: thick gel
Compositions 11C
Figure BPA00001701982701382
Figure BPA00001701982701391
Goal standard 11C:
pH:5.00-6.50
Viscosity (RV T-B, 10rpm, 1min, 25 ℃): 5,000-15,000cps
Color: translucent white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, Lac Bovis seu Bubali shape liquid
Compositions 11D
Figure BPA00001701982701392
Figure BPA00001701982701401
Figure BPA00001701982701411
Goal standard 11D:
pH:4.50-6.00
Viscosity (RV T-B, 10rpm, 1min, 25 ℃): 20,000-30,000cps
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: the opaque emulsion of thickness
Compositions 11E
Figure BPA00001701982701412
Figure BPA00001701982701421
Goal standard 11E:
pH:6.5-7.5
Viscosity (RV T-B, 10rpm, 1min, 25 ℃): 5,000-15,000cps
Color: colourless-faint yellow
Abnormal smells from the patient: MS
Outward appearance: the oil-based liquid of slight haze
Compositions 11F
Figure BPA00001701982701431
Figure BPA00001701982701441
Goal standard 11F:
pH:6.5-7.5
Viscosity (RV T-C, 5rpm, 1min, 25 ℃): 50,000-100,000cps
Color: colourless-faint yellow
Abnormal smells from the patient: MS
Outward appearance: the tacky wax of slight haze
Compositions 11G-1 to 11G-4
Figure BPA00001701982701442
Figure BPA00001701982701451
Figure BPA00001701982701461
Goal standard, body:
pH:5.0-6.5
Color: cream-coloured (MS)
Abnormal smells from the patient: MS
Outward appearance: troubled liquor
Goal standard, finished product:
pH:5.0-6.5
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: dense foam, non-water sample, do not trickle
Foam stability: 200 seconds minutes
Spray diameter (8 "): foam
Spray pattern (8 "): foam
Table 13
Figure BPA00001701982701462
Figure BPA00001701982701471
Table 14
Figure BPA00001701982701472
Embodiment 12
The present embodiment has illustrated that compositions of the present invention has alleviated the situation that hair is died down due to the fomentation plate.
Comparative composition 12A
Figure BPA00001701982701473
Figure BPA00001701982701481
Goal standard 12A:
pH:6.0-7.0
Viscosity (RV T-C, 5rpm, 1min, 25 ℃): 40,000-80,000
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque (muddy) gel
Comparative composition 12B
Component % by weight
Water (Aqua, Eau) 39.52699
Aminomethyl propanol, water (approximately 5% water) 0.02
Acrylic acid/VP cross linked polymer 1
Water (Aqua, Eau) 23.2
Aminomethyl propanol, water (approximately 5% water) 0.44
Water (Aqua, Eau) 20
Water (Aqua, Eau) 0.013
Dyestuff 0.000013
Polyquaternary ammonium salt-4 0.5
EDETATE SODIUM 0.05
PVP (20%), water (Aqua, Eau) 4
VP/ Methacrylamide/vinyl imidazole copolymer (approximately 20%), water 3.5
Polyquaternary ammonium salt-39 (8.58%), water 0.5
Propylene glycol 1
Sorbitol, water (30% water) 0.5
Aminomethyl propanol, water (approximately 5% water) 0.15
Water (Aqua, Eau) 4.8
Oleth-20 0.45
Flavouring agent 0.15
DMDM Hydantoin (55%), water 0.2
In the compound container of main rustless steel, (turbine-type mixer is with strong counter clockwise direction under strong stirring; Side is swept blender with on moderate clockwise direction), add the cold water of 68-86 ℉ (20-86 ℃).
The first aminomethyl propanol (AMP-95) is added into main clad vessel, and mixes until disperse fully.
Next, under strong stirring (in the situation that possible be eddy current; Turbine-type mixer is with strong counter clockwise direction; Side is swept blender with on moderate clockwise direction) lentamente acrylic acid/VP crosslinked polymer powder is sprayed in main clad vessel.Ejector pump or arbitrarily other online disperser can be used for this interpolation.Careful operation during adding powder will be lumpd because if add too fast words.Batch mixture at least 45 minutes or until polymer disperses fully and no longer exists granule or piece.When mixing, begin to prepare the Celquat premix.
Disperseed and no longer had granule or a piece from the sampling of main clad vessel and all polymer of visual examination.Still exist as fruit granule or piece, continue so strong mixing and periodically again sub-sampling until batch of material is even.
Next, after disperseing Visual Confirmation, (turbine-type mixer is with moderate counter clockwise direction under moderate stirring; Side sweep blender with slowly clockwise on) deionized water is filled to main clad vessel.Careful operation when filled with water, and slow down and mix to avoid inflation.The filling of this water should make the level of batch of material higher than the top of blade, thereby avoids splashing and inflating in the neutralization procedure process.Batch mixture at least 15 minutes or until batch of material is smooth and uniform.
In case batch of material is even after deionized water filling, continue to mix that (turbine-type mixer is with moderate counter clockwise direction moderately; Side is swept blender with on moderate clockwise direction), and with the second aminomethyl propanol (AMP-95) be added in main clad vessel with in and polymer.Solution will become clarification at last, and viscosity will sharply increase.Batch mixture at least 20 minutes or until batch of material is uniform.
In suitable rustless steel premixing container, load the following cold water that is set in 68-86 ℉ (20-30 ℃).(if feasible, turbine-type mixer is with strong counter clockwise direction to begin strong mixing; Side is swept blender with on moderate clockwise direction).
In suitable rustless steel container, in the situation that feasible, with the dyestuff premixing in the warm water that is set in 104-113 ℉ (40-45 ℃).Mix until dyestuff fully dissolves and evenly.Mix until premix evenly and not contains any undissolved granule.In case the dyestuff premix is ready to, this solution is added into the phase container.
Next, under strong stirring (in the situation that possible be eddy current; Turbine-type mixer is with strong counter clockwise direction; Side is swept blender with moderate clockwise direction) lentamente polyquaternary ammonium salt-4 powder is sprayed in the phase container.Ejector pump or any other online disperser can be used for this interpolation.Careful operation during adding powder will be lumpd because if add too fast words.Batch mixture at least 30 minutes or until no longer have granule or piece.
Disperseed and do not had granule or a piece from phase container sampling and all polymer of visual examination.Still exist as fruit granule or piece, continue strong mix and periodically again sub-sampling until batch of material is even.
In case be mutually clarification and uniform, (if feasible, turbine-type mixer is with strong counter clockwise direction following component to be added into the premixing container; Side is swept blender with moderate clockwise direction): EDETATE SODIUM; PVP K-90 (20% solution); VP/ Methacrylamide/vinyl imidazole copolymer; Polyquaternary ammonium salt-39; Propylene glycol; Sorbitol; Aminomethyl propanol.
In case premix is ready to, it is added in main clad vessel.With the cold rinse premixing container that is set in 68-86 ℉ (20-30 ℃), and it is added into main clad vessel, and (turbine-type mixer is with moderate counter clockwise direction; Side is swept blender with moderate clockwise direction).Batch mixture at least 20 minutes or until batch of material is even.
The flavouring agent premix that is prepared as follows in the container of suitable, the cleaning that disposes electronic or air mixer: oleth-20; Flavouring agent.For evenly and be easy to process, oleth-20 should be in the lower pre-fusion of 95-104 ℉ (35-40 ℃).If it is higher than 110 ℉ (43 ℃) this component is not mixed mutually with flavouring agent, otherwise flavouring agent will be flashed out.Mix consumingly this premix until its for clarification and do not contain any undissolved material.Visual examination its for clarification and do not contain granule, and then it is added into main clad vessel under moderate stirring.
Check that batch temperature is 104 ℉ (40 ℃) or lower (if necessary cooling batch of material), and then (turbine-type mixer is with moderate counter clockwise direction under moderate stirring; Side is swept blender with on moderate clockwise direction) DMDM Hydantoin is added in main clad vessel.Mixed at least 30 minutes or until batch of material is fully even.Compositions is taken a sample.Stop mixing and cooling (if feasible).
Can followingly regulate.If pH is low, 5% add aminomethyl propanol take maximum as total batch of material demand.If pH is high, 0.1% citric acid that adds at first premixing in water (20% solution) take maximum as total batch of material.If viscosity is low, mixed extra 60 minutes and sub-sampling again.Should comprise air film type and positive displacement type for the pump of material pump being delivered to container.The filter that should use comprises 80 orders for all conveying operations.Filling temp should be 68-95 ℉ (20-35 ℃).
Compositions 12C
Figure BPA00001701982701521
Figure BPA00001701982701531
Goal standard 12C:
pH:6.0-7.0
Viscosity (RVT-C, 5rpm, 1min, 25 ℃): 40,000-80,000
Color: white (MS)
Abnormal smells from the patient: MS
Outward appearance: thickness, opaque (muddy) gel
Comparative composition 12D: the Rhodapex ES-2 (sodium laureth sulfate) from Rhodia is diluted with water to 12% active component.
The quantification of fibre debris:
Have one's hair wash with sodium laureth sulfate.
The test material of scheduled volume is applied to moist hair and evenly distributes.
In the situation that not combing dries up topknot.
Ironing under 205 ℃.Approximately ironing board is being pulled to the bottom from the top of topknot in 12 seconds; Repeat 5 times, total time is 1 minute.Make topknot cooling.Repeat to implement 3 other (4 minutes altogether) of heat treatment.
Repeat all above-mentioned steps three times.
Utilize the sodium laureth sulfate hair washing.
Dry up the w/o combing
Translucent plastics are placed under topknot.
Utilize five stripping fork combings 100 times (be actually and knock, namely knock speed).
Tape on plastics with fastening fragment.
To all collected hair fragment numberings.
Calculate the percentage ratio that hairs break (protection) reduces:
Hairs break reduces %=[(C-T)/C] * 100
The number of the hair fragment that is used for contrast that C=is collected
The number of the hair fragment that is used for test that T=is collected
The equipment that is used for tryptophan degraded spectrofluorometry is Spectrofluorimeter-Horiba Jobin Yvon FluoroMax 4.Test in the high window of the wide and 1.7cm of 2.3cm the top that is positioned at topknot or five different positions of root carry out, the topknot from the bottom of bonding topknot to the intermediate point of window is 2 inches.Being set as of equipment in test process:
Excite: the 290nm wavelength; The 5mm slit
Emission: from 300-400nm; The 5mm slit; The 1nm increment comes record from the measurement of the emission spectra of 300-400nm with the increment of 1nm.Then average five measurements at the 336nm place (maximum point of tryptophan emission).Calculate to initial reading and after the flat process of fomentation.The degraded percentage calculation is as follows:
[(before processing after 5 emission reading meansigma methods-processing of 336nm in 5 emission reading meansigma methodss of 336nm)/before processing launches the reading meansigma methodss 5 times of 336nm] * 100%
The protection percentage calculation is as follows:
[the degraded % of (the degraded % of the degraded %-test of contrast)/contrast] * 100%
Damp condition: topknot is overnight storage (76 ℃ of dry bulb formulas under 22%RH; 54 ℃ of wet bulb formulas).(75 ℃ of dry bulb formulas are carried out in the combing test at 30%RH; 56 ℃ of wet bulb formulas).
Table 15 and 16 has shown the resisting breakage data.Table 15 has shown the numerical value of hair fragment.Table 16 has shown that the breakage with respect to compositions 12D reduces percentage ratio.
Table 15
Situation Topknot 1 Topknot 2 Topknot 3 Topknot 4 Topknot 5
12A 352 338 408 202 140
12B 327 294 241 272 172
12C 154 82 157 121 128
12C 412 503 234 289 342
Table 16
Situation Meansigma methods (n=5) Standard deviation Reduction % with respect to 12D
12A 288.0 112.1 19.1
12B 261.2 58.9 26.6
12C 128.4 30.3 63.9
12D 356.0 105.3
Fig. 8 has shown the heat protection percentage ratio by tryptophan measurement.Compositions 12C has reduced the tryptophan degraded significantly.And the trend of tryptophan percent loss is relevant well to the quantification of fibre debris.
The present embodiment illustrates the gel that contains PEC and has reduced significantly the fibre debris of combing generation and the percentage ratio of tryptophan loss.
Embodiment 13
The present embodiment has illustrated the freeze-thaw stability of exemplary composition of the present invention.
Compositions 13A-13D
Figure BPA00001701982701551
Figure BPA00001701982701571
Compositions 13E-13G
Figure BPA00001701982701581
Figure BPA00001701982701591
Figure BPA00001701982701592
Compositions 13H-13K
Figure BPA00001701982701593
Figure BPA00001701982701611
Compositions 13L-13N
Figure BPA00001701982701612
Figure BPA00001701982701621
Figure BPA00001701982701631
Figure BPA00001701982701632
Compositions 13O-13R
Figure BPA00001701982701633
Figure BPA00001701982701641
Figure BPA00001701982701651
Compositions 13S-13V
Figure BPA00001701982701671
Compositions 13W-13Z
Figure BPA00001701982701672
Figure BPA00001701982701681
Compositions 13AA-13CC
Figure BPA00001701982701692
Figure BPA00001701982701701
Compositions 13DD-13EE
Figure BPA00001701982701712
Figure BPA00001701982701731
Figure BPA00001701982701732
Figure BPA00001701982701741
Compositions 13FF-13HH
Figure BPA00001701982701742
Figure BPA00001701982701751
Figure BPA00001701982701761
Compositions 13II-13LL
Figure BPA00001701982701762
Figure BPA00001701982701771
Figure BPA00001701982701781
Figure BPA00001701982701782
The process of freezing/melting stability study is as follows:
1, fill finished product in vial.If testing package is stable, just product is filled in the container of suitable packing.
2, bottle and the packing filled after, each is carried out labelling.Tape to guarantee that they remain on appropriate position in whole stability study around labelling.
Before in being placed on cryoprobe, record initial pH, viscosity, outward appearance, color and the abnormal smells from the patient of batch of material.
3, all bottle/packings are placed in cryoprobe 24 hours.
4, took a sample from cryoprobe after 24 hours, and they are placed in material box on stand or on napkin.Described sample was thawed 24 hours.
5, outward appearance, color and the abnormal smells from the patient of sample for reference after other 24 hours.If feasible, measure pH and viscosity.Record result.
Measure viscosity with following parameter: RV, T-bar B, 10rpm, 60 seconds, 25 ℃ when surpassing 40,000cps (except when, method is RV, T-bar C, 5rpm, 60 seconds, 25 ℃).
Table 17-20 has shown viscosity (cps) and the pH reading of several compositionss as implied above.
Table 17
13A 13B 13C 13D 13E 13F 13G
Initially pH 4.92 4.94 4.88 4.79 4.69 4.77 4.75
Viscosity 22,000 20,000 19,600 18,200 15,600 16,800 19,200
24 hours pH 4.90 4.91 4.86 4.77 4.73 4.73 4.81
Viscosity 25,200 24,800 23,600 19,600 22,800 29,600 31,600
Table 18
13I 13J 13K 13L 13M 13N
24 hours pH 4.90 4.87 4.93 4.86 5.04 4.90
Viscosity 20,600 22,000 26,400 23,600 28,400 35,600
Table 19
Figure BPA00001701982701791
Figure BPA00001701982701801
N/a=is greater than 1MM
Table 20
Figure BPA00001701982701802
About compositions 13O-13R,
Figure BPA00001701982701803
The recommended amounts of SC-96: use 1-5% for 13O, use 0.5-3% for 13P, use 2-10% for 13Q, use 2-12% for 13R.
Fig. 9 has shown to measure to have the compositions 13H-13J of different dihydroxylic alcohols and the comparative result that freezes/melt stable effectiveness of 13EE.Compositions 13H does not show freeze-thaw stability.The propylene glycol (compositions 13I) of interpolation 5% does not greatly improve and freezes/melt stability.Add 10% propylene glycol (compositions 13J) or spermol is reduced to 1% and contain
Figure BPA00001701982701804
SC-96 (compositions 13EE) shows and freezes/melt stability.
Figure 10 has shown the comparison of compositions 13K-13N.Different dihydroxylic alcohols, for example glycerol and sorbitol freeze/melt on stability effective like that not as propylene glycol in improvement.
Figure 11 has shown the comparison of compositions 13A-13C.Compound polyelectrolyte being reduced to 1% having shown the more not serious unstability of freezing/melt, is not optimum (13A is to 13H) but freeze/melt stability.5% propylene glycol (13B) demonstrates some improvement; 10% (13C) demonstrates positive result.
Figure 12 has shown the comparison of compositions 13D-13G.Add glycerol and sorbitol not to demonstrate and freeze/melt stability, even also do not have when compound polyelectrolyte is reduced to 1%.
Figure 13 has shown the comparison of compositions 13S-13U.Compound polyelectrolyte has been added into Emulsion " destruction " viscosity (13S (there is no PEC) contrast 13T (containing PEC) contrast 13U (containing PEC)).(13U) interpolation polyelectrolyte is slightly lower with respect to the effect of adding (13T) before completing after breast is completed mutually.
Figure 14 has shown the comparison of compositions 13V-13X.Add before or after Emulsion compound polyelectrolyte and the time (13W and 13X contrast 13T and 13U), add Salcare at breast before mutually SC-96 can be used for thickening Emulsion.Yet the low and final viscosity of initial viscosity will spend 72 hours and set up, and this is not preferred in production environment.And 13X is not preferred in production environment, because batch of material is too thick and be difficult to mixing (not having extra water and PEC to reduce the viscosity of batch of material) in newborn phase process.Freezing/melt stability and spreadability can improve by adding propylene glycol or Crodamol STS.
Figure 15 has shown the comparison of compositions 13FF-13HH.Add propylene glycol and Crodamol STS and can not adversely affect emulsion viscosity (13V, 13W, 13X have similar result, except initial viscosity thicker).13GG can be used as the candidate of single container technique, yet its final viscosity is lower than 13DD/13KK.13HH is not still preferred aborning, because batch of material is too thick in newborn phase process.
Figure 16 has shown the comparison of compositions 13Y-13AA.When adding compound polyelectrolyte before or after emulsion, (13Z and 13AA contrast 13T and 13U), add after the breast phase
Figure BPA00001701982701811
SC-96 can be used for thickening emulsion.13AA is preferred with respect to 13X from the angle of producing, because batch of material is not too thick and can be mixed rightly.For thick finished product, compound polyelectrolyte can add (13AA is to 13Z) after emulsion.Be similar to 13W and 13X, freezing/melt stability and spreadability can improve by adding propylene glycol or Crodamol STS.
Figure 17 has shown the comparison of compositions 13II-13KK.Add propylene glycol and Crodamol STS and improved initial and final Emulsion viscosity (13JJ and 13KK contrast 13Z and 13AA).It is not preferred adding complex before Emulsion, because viscosity rare (13JJ contrasts 13KK).
Figure 18 has shown the comparison of compositions 13BB-13DD.Propylene glycol and Crodamol STS have both increased viscosity individually and jointly.
Figure 19 has shown the comparison of compositions 13EE and 13LL.If spermol is reduced to 1% and Salcare SC-96 increases to 5% (13EE), can remove Crodamol STS and propylene glycol.Do not comprise spermol generate lack basic " conditioner characteristic " product (opacity, Emulsion body) (13LL).
Embodiment 14
The present embodiment has illustrated the furcated end reparation of exemplary composition of the present invention.
Compositions 14A
The Gantrez AN-119 of I, preparation 2% active component
The A part
Describe
Deionized water 94.4
20%NaOH 3.6
GANTREZ S-97BF polymer 2
If necessary, utilize NaOH to regulate pH to 6.95+/-0.05.
II, the preparation 2% active component polyquaternary ammonium salt-28
The B part
Describe
Deionized water 90.25
CONDITIONEZE NT-20 9.755
III, merging A﹠amp; B (complex concentrate)
The C part
Describe
The A part 5
The B part 45
IV, preparation conditioner preparation
The D part
Describe
Begin to be heated to 75-80 ℃
Deionized water 39.67
L-Aspartic acid 0.8
Hydroxyethyl-cellulose 0.5
Xanthan gum 0.05
EDETATE SODIUM 0.03
The complex concentrate ( *The C part) 50.1
In the following component to 80 of independent vessel in heating ℃
Spermol 5
SAPDMA 2
Glyceryl stearate 0.2
Then return and add to water and mix under 75-80 ℃
Add;
Cocamido propyl betaine 1
Be cooled to 45 ℃, then add remaining component
DMDM 0.2
Flavouring agent 0.45
Utilize citric acid to be adjusted to approximately pH=5
The compositions of being somebody's turn to do " not containing complex " as above prepares, but utilizes water to replace the C part.Contrast is the anti-damage conditioner of Tresemme (Tresemme Anti-Breakage Conditioner).
Method: use five 1 " wide, that bleached, impaired topknot (from Int ' 1 Hari Importers), cut 10 fibers and labelling rightly from each sample with furcated end.Gather original photo at microscopically.Application standard step hair washing (1 " use 1mL on topknot, time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds, 35-40 ℃ of water temperature, the speed of 2gal/min).Conditioning (1 " use 1mL on topknot, time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds, 35-40 ℃ of water temperature, the speed of 2gal/min).Use wide increment combing to wet and send out once, use narrow another time of end combing.Dry up under high heat, until bone dry, and then combing twice, wide increment once used, and narrow increment is used in another time.The calculating quantity that fiber is repaired after for the third time with six processing.Gather final photo.
Calculate:
Repair the fiber number of the fiber sum cut before %=[(processes-disconnect after processing)-quantity of furcated end after processing]/(the fiber sum of cutting before processing-disconnect after processing fiber number)
Disconnect %=100 * (the fiber sum of cutting before the fiber number of disconnection/processing)
Table 21 has shown this result.
Table 21
Figure BPA00001701982701841
Embodiment 15
The present embodiment has illustrated the furcated end reparation of exemplary composition of the present invention.
Compositions 15A-15D
Compositions 15A 15B 15C 15D
PEC% 0.5 1 2 3
The Gantrez AN-119 of I, preparation 4% active component
The A part
Figure BPA00001701982701842
The polyquaternary ammonium salt-28 of II, preparation 4% active component
The B part
III, merging A﹠amp; B (complex concentrate)
The C part
Figure BPA00001701982701852
IV, preparation conditioner preparation
The D part
Figure BPA00001701982701861
Compositions 15E
The Gantrez AN-119 of I, preparation 4% active component
The A part
Figure BPA00001701982701862
The polyquaternary ammonium salt-28 of II, preparation 4% active component
The B part
Describe
Deionized water 80.49
CONDITIONEZE NT-20 19.51
III, merging A﹠amp; B (complex concentrate)
The C part
Describe
The A part 5
The B part 45
IV, preparation conditioner formula
The D part
Figure BPA00001701982701863
Figure BPA00001701982701871
Test 1
From 1 " wide brown topknot, cut the fiber with furcated end and gather initial photo.With contrast shampoo (the Alberto VO5 Normal shampoo) bundle of having one's hair wash respectively, carry out afterwards corresponding conditioner and process.Repeated washing at least twice.Dry up topknot and air drying 24 hours.Gather the final photo of each fiber of cutting.
Test 1 result is shown in Figure 20, following processing shown in it:
Fiber 1 on topknot 1: use water treatment
Fiber 2 on topknot 2: contrast shampoo-contrast VO5 adds health conditioner (Body Conditioner)
Fiber 3 on topknot 3: contrast shampoo-compositions 15C
Fiber 4 on topknot 3: contrast shampoo-compositions 15C
Test 2
From 1 " wide brown topknot, cut five and have the fiber of furcated end and gather initial photo.With the contrast shampoo bundle of having one's hair wash respectively, carry out afterwards corresponding conditioner and process.(according to standard wash program: 1mL, 1min time of contact, rinsing in 20 seconds, 35-40 ℃ of water temperature).Under the speed of 2gal/min, a topknot is used compositions 15E, and another topknot uses compositions 15C.Repeated washing at least twice.Dry up topknot and air drying 24 hours.Gather the final photo of each fiber of cutting.
Do not provide too many conditioning benefit by adding siloxanes, but the reparation of furcated end is still significantly.
Test 3
Use three 1 " wide brown topknot, cut 10 fibers with furcated end and labelling rightly from each sample.Application standard program hair washing bundle (1 " use 1mL on topknot, time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds, 35-40 ℃ of water temperature, the speed of 2gal/min).With compositions 15C conditioning (1 " use 1mL on topknot, time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds, 35-40 ℃ of water temperature, the speed of 2gal/min).Use wide increment combing to wet and send out once, and use narrow another time of end combing.Combing twice again after drying up once use wide increment, and narrow increment is used in another time.Repeat as required above-mentioned steps.Calculate the fiber number of repairing after each the processing.
Result is shown in table 22.
Table 22
Number of processes 1 2 3 4 5 6 7 8 9 10
Repair percentage ratio 17% 26% 57% 57% 57% 57% 61% 61% 61% 61%
Test 4
Use five 1 " topknot wide bleaching, impaired (from Int ' 1 Hair Imports), cut 10 fibers with furcated end and labelling rightly from each sample.At the initial photo of microscopically collection.Application standard program hair washing bundle (1 " use 1mL on topknot, time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds, 35-40 ℃ of water temperature, the speed of 2gal/min).Conditioning (1 " use 1mL on topknot, time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds, 35-40 ℃ of water temperature, the speed of 2gal/min).Use wide increment combing to wet and send out once, and use narrow another time of end combing.Dry up under high heat until bone dry, and then combing twice, wide increment once used, and narrow end is used in another time.For the third time, the 6th time and the tenth time calculate the quantity of reparation fiber after processing.Gather final photo.
Calculate
The initial number of the furcated end fiber of the quantity of furcated end after repairing %=100* and processing/cut
The initial number of the furcated end fiber of cutting before the fiber number that disconnection %=100* disconnects/processing
Result is shown in table 23.
Table 23
The fabulous conditioning that compositions 15C provides the topknot of bleaching, and be easy to wet combing.
Test 5
The each processing used two 1 " topknot wide bleaching, impaired.Cut 10 fibers with furcated end and labelling rightly from each sample.At the initial photo of microscopically collection.The Application standard program have one's hair wash respectively bundle (1 " use 1mL on topknot, time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds, 35-40 ℃ of water temperature, the speed of 2gal/min).With compositions 15B, 15C or 15D nurse one's health respectively topknot (1 " use 1mL on topknot, time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds, 35-40 ℃ of water temperature, the speed of 2gal/min).Use wide increment combing to wet and send out once, and use narrow another time of end combing.Dry up under high heat until bone dry, and then combing twice, wide increment once used, and narrow end is used in another time.Calculate the quantity of repairing fiber after the processing of suitable number of times.Gather final photo.
Result is shown in table 24.
Table 24
Figure BPA00001701982701901
Test 6
Use three 1 " wide brown topknot, cut 10 fibers with furcated end and labelling rightly from each sample.The Application standard program have one's hair wash respectively bundle (1 " use 1mL on topknot, time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds, 35-40 ℃ of water temperature, the speed of 2gal/min).With contrast 1 (Nexxus commercial preparation), contrast 2, compositions 15A, 15B, 15C or 15D nurse one's health respectively topknot (1 " use 1mL on topknot; time of contact 1min, every side is knocked for 10 times, rinsing in 20 seconds; 35-40 ℃ of water temperature, the speed of 2gal/min).Use wide increment combing to wet and send out once, and use narrow another time of end combing.Combing twice again after drying up once use wide increment, and narrow end is used in another time.Repeat as required above-mentioned step.Calculate the quantity of repairing fiber after each the processing.Calculate the quantity that disconnects fiber after each the processing.
Contrast 2 compositionss
Describe
Begin to be heated to 75-80 ℃
Deionized water 89.77
L-Aspartic acid 0.8
Hydroxyethyl-cellulose 0.5
Xanthan gum 0.05
EDETATE SODIUM 0.03
In the following component to 80 of independent vessel in heating ℃
Spermol 5
SAPDMA 2
Glyceryl stearate 0.2
Be added into afterwards water and mixed 15 minutes under 75-80 ℃
Add;
Mackam CB35 (coco betaine) 1
Be cooled to 45 ℃, add afterwards remaining component
DMDM 0.2
Flavouring agent 0.45
Be adjusted to approximately pH=5 with citric acid
Specification
pH 4.35
Viscosity (RVT-B, 10rpm, 1min, 25 ℃) 4,800
Result is shown in table 25 and 26.
Table 25
Figure BPA00001701982701911
Table 26
Figure BPA00001701982701912
Embodiment 16
The present embodiment has illustrated the furcated end reparation of exemplary composition of the present invention.
Compositions 16A
Figure BPA00001701982701921
Blend step:
1, premixing-adding ingredient #1-2 also mixes until hydration
2, with composition #3 with pH regulator to 6.9-7, then be heated to 50-55 ℃
3, adding ingredient #4 lentamente under very strong mixing mixed approximately 10 minutes
4, in primary tank, adding ingredient #5 also begins to be heated to 80-85 ℃
5, adding ingredient #6-7.When batch of material reaches 80 ℃, add #8-10 and mixed 30 minutes.
6, begin to cool down batch of material, when lower than 45 ℃, add premix and remaining ingredient from step 1-3.
Goal standard:
The liquid of outward appearance-opaque, thickness
Abnormal smells from the patient-match-on criterion
pH-4.5-5.5
Viscosity-10,000-15,000cps RTV-B 10rpm, 60 seconds
Comparative composition 16B
Figure BPA00001701982701931
Figure BPA00001701982701941
Blend step:
1, in primary tank, adding ingredient #1-2 also begins to be heated to 80-85 ℃
2, adding ingredient #3 when not having piece
3, when 1-3 does not have piece, continue to be heated to 80-85 ℃
4, when batch of material reaches 80-85 ℃, adding ingredient #4-17 also mixed 30 minutes
5, begin to cool down batch of material, when lower than 45 ℃, add 11-18
Goal standard:
The liquid of outward appearance-opaque, thickness
Abnormal smells from the patient-match-on criterion
pH-4.5-5.5
Viscosity-10,000-15,000cps RTV-810rpm, 60 seconds
Compositions 16A has 4.92 pH and the viscosity of 10,800cps.Compositions 16B has 4.95 pH and the viscosity of 7,200cps.
When comparing, the wet and dried combing of compositions 16A is far better.
The topknot of twice bleaching is thumped to be added and dries up, to produce furcated end.Cut ten furcation areas in every four 11/2 inch wide topknots.Then two topknots are washed and use compositions 16A to nurse one's health with Alberto VO5 Normal shampoo.Two topknots are washed and use comparative composition 16B to nurse one's health with Alberto VO5 Normal shampoo.
Compositions 16A provides 90% furcated end reparation, and comparative composition 16B provides 63% furcated end reparation.N-Hance SP-100 is added into the repair ability that formula has improved final preparation.
All lists of references of quoting at this paper, comprise publication, patent application and patent, thus by with reference to being incorporated into such degree, as having pointed out that separately and especially every piece of document all incorporates into by reference, and all propose in this article with it.
The term " one " of the use of (in the context of claim especially below) and " one " and " described/should " and similar attribute should be interpreted as having covered odd number and plural number both in describing context of the present invention, unless be otherwise noted in this article or obvious and contradicted by context.Term " comprises ", " having ", " comprising " and " containing " should be interpreted as open term (namely meaning " including but not limited to "), except as otherwise noted.Numerical range described herein only is intended to the method for simplifying that falls into each the independent numerical value in this scope as quoting separately, unless this otherwise noted, and each independent numerical value all is merged in description, is documented in herein separately as it.All methods described herein can be carried out with any suitable order, unless this otherwise noted, perhaps obviously and contradicted by context.Any and all embodiment provided herein, the perhaps use of exemplary term (for example " for example "), only intention is used for the present invention being described better and the scope of the invention not being limited, except as otherwise noted.Term in this manual should not be interpreted into the key element of pointing out to implement the necessary any undesired protection of the present invention.
This paper describes the preferred embodiment of the present invention, comprise that known being used for of applicant implement best mode of the present invention.For a person skilled in the art, after the description of having read the front, obviously can obtain the distortion of these preferred implementations.The inventor estimates that those skilled in the art take the circumstances into consideration to adopt these distortion, and the inventor plans to implement the present invention except clearly describing herein.Therefore, the present invention includes all modifications and the equivalent variations of the theme of putting down in writing in additional claims by allowing in applicable law.In addition, in its described possible distortion, any combination of above-described element all is included in the present invention, unless this otherwise noted or obvious and contradicted by context.

Claims (12)

1. hair care composition, it comprises:
Compound polyelectrolyte, it comprises cation type polymer and anionic polymer;
Approximately 3% to about 5% thickening agent; And
Approximately 2% or emollient still less;
Percentage ratio wherein is based on the gross weight meter of compositions.
2. the compositions of claim 1, wherein, described thickening agent comprises quaternary nitrogen compound or quaternary nitrogen polymer.
3. the compositions of claim 2, wherein, described quaternary nitrogen polymer is polyquaternary ammonium salt-37.
4. the compositions of claim 3, wherein, described polyquaternary ammonium salt-37 are the mixture with propylene glycol dicaprylate/dicaprate and polypropylene glycol-1 tridecyl alcohol polyethers-6.
5. the compositions of claim 1, wherein, described emollient is aliphatic alcohol.
6. the compositions of claim 5, wherein, described aliphatic alcohol is spermol, stearyl alcohol or its combination.
7. the compositions of claim 1, wherein, the consumption of described compound polyelectrolyte is based on approximately 1% to approximately 8% of the gross weight of compositions.
8. the compositions of claim 7, wherein, the consumption of described compound polyelectrolyte is based on approximately 1% to approximately 3% of the gross weight of compositions.
9. the compositions of claim 1, wherein, described cation type polymer comprises one or more monomeric units with one or more quaternary nitrogen groups.
10. the compositions of claim 9, wherein, described cation type polymer is polyquaternary ammonium salt-28.
11. the compositions of claim 1, wherein, described anionic polymer comprises the monomeric unit with ionizable hydroxy-acid group.
12. the compositions of claim 11, wherein, described anionic polymer is methyl vinyl ether/maleic acid.
CN201180051080.8A 2010-10-20 2011-10-07 Hair maintenance compositions and correlation technique Active CN103179943B (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US39496610P 2010-10-20 2010-10-20
US61/394,966 2010-10-20
PCT/US2010/053360 WO2012054029A1 (en) 2010-10-20 2010-10-20 Hair-mending compositions and associated methods
USPCT/US10/053360 2010-10-20
PCT/US2011/055370 WO2012054243A2 (en) 2010-10-20 2011-10-07 Hair-mending compositions and associated methods

Publications (2)

Publication Number Publication Date
CN103179943A true CN103179943A (en) 2013-06-26
CN103179943B CN103179943B (en) 2015-12-16

Family

ID=45975511

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201180051080.8A Active CN103179943B (en) 2010-10-20 2011-10-07 Hair maintenance compositions and correlation technique

Country Status (8)

Country Link
EP (1) EP2629742A4 (en)
JP (1) JP5977750B2 (en)
CN (1) CN103179943B (en)
BR (1) BR112013009589A2 (en)
CA (1) CA2812991C (en)
EA (1) EA024282B1 (en)
MX (1) MX350219B (en)
WO (2) WO2012054029A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107519031A (en) * 2016-06-21 2017-12-29 强生消费者公司 personal care composition containing complexing polyelectrolyte

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012075274A1 (en) * 2010-12-01 2012-06-07 Isp Investments Inc. Durable styling compositions and the uses thereof
WO2014020081A2 (en) * 2012-08-03 2014-02-06 Unilever Plc Composition
US20160008257A1 (en) * 2013-03-15 2016-01-14 Isp Investments Inc. Hair care compositions containing polyelectrolyte complexes
DE102013224868A1 (en) * 2013-12-04 2015-06-11 Henkel Ag & Co. Kgaa Styling agent with high curl retention
JP2015107939A (en) * 2013-12-05 2015-06-11 ロレアル Cosmetic treatment method
JP6993114B2 (en) * 2017-06-13 2022-01-13 株式会社ミルボン Cosmetic composition
FR3090366B1 (en) * 2018-12-21 2021-06-04 Oreal Composition Comprising at least one Vinyl Lactam (Meth) Acrylic Copolymer, at least two Amino Silicones and at least one Solvent
US20220273554A1 (en) * 2019-09-30 2022-09-01 Kao Corporation Cleaning agent
EP4039336A4 (en) * 2019-09-30 2023-11-29 Kao Corporation Detergent
FR3108510A1 (en) * 2020-03-26 2021-10-01 L'oreal Composition comprising a positively charged polyion complex
WO2021171909A1 (en) * 2020-02-26 2021-09-02 L'oreal Composition comprising positively charged polyion complex
JP2023553501A (en) * 2020-12-16 2023-12-21 ロレアル Compositions for caring for the skin
FR3140272A1 (en) * 2022-09-30 2024-04-05 L'oreal Cosmetic hair care composition comprising particular amino silicones and perfuming substances, and method for cosmetic treatment of hair.
FR3140280A1 (en) * 2022-09-30 2024-04-05 L'oreal Cosmetic hair care composition comprising at least one particular amino silicone and at least one polyol, and cosmetic treatment method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060188468A1 (en) * 2003-07-14 2006-08-24 Basf Aktiengesellschaft Cosmetic and pharmaceutical substances based on polyelectrolyte complexes
US20060251603A1 (en) * 2004-07-14 2006-11-09 Isp Investments Inc. Mending hair damage with polyelectrolyte complexes
CN1890277A (en) * 2003-12-09 2007-01-03 巴斯福股份公司 Ampholytic anionic copolymers
CN101395202A (en) * 2006-03-03 2009-03-25 帝斯曼知识产权资产管理有限公司 Hair care compositions

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
LU76955A1 (en) * 1977-03-15 1978-10-18
US4299817A (en) * 1977-08-24 1981-11-10 Union Carbide Corporation Hair care compositions
LU84708A1 (en) * 1983-03-23 1984-11-14 Oreal THICKENED OR GELLIED HAIR CONDITIONING COMPOSITION CONTAINING AT LEAST ONE CATIONIC POLYMER, AT LEAST ONE ANIONIC POLYMER AND AT LEAST ONE XANTHANE GUM
LU86429A1 (en) * 1986-05-16 1987-12-16 Oreal COSMETIC COMPOSITIONS CONTAINING A CATIONIC POLYMER AND AN ANIONIC POLYMER AS A THICKENING AGENT
US20050089494A1 (en) * 2003-10-28 2005-04-28 Isp Investments Inc. Mending hair damage with polyelectrolyte complexes
EP1779838A1 (en) * 2005-10-26 2007-05-02 KPSS-Kao Professional Salon Services GmbH Hair conditioning composition comprising Polyquaternium 37, fatty alcohol and non-ionic / cationic surfactant
JP5461847B2 (en) * 2009-02-13 2014-04-02 花王株式会社 Hairdressing composition

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060188468A1 (en) * 2003-07-14 2006-08-24 Basf Aktiengesellschaft Cosmetic and pharmaceutical substances based on polyelectrolyte complexes
CN1890277A (en) * 2003-12-09 2007-01-03 巴斯福股份公司 Ampholytic anionic copolymers
US20060251603A1 (en) * 2004-07-14 2006-11-09 Isp Investments Inc. Mending hair damage with polyelectrolyte complexes
CN101395202A (en) * 2006-03-03 2009-03-25 帝斯曼知识产权资产管理有限公司 Hair care compositions

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107519031A (en) * 2016-06-21 2017-12-29 强生消费者公司 personal care composition containing complexing polyelectrolyte

Also Published As

Publication number Publication date
WO2012054243A2 (en) 2012-04-26
EP2629742A2 (en) 2013-08-28
EP2629742A4 (en) 2015-12-16
EA024282B1 (en) 2016-09-30
MX350219B (en) 2017-08-30
CN103179943B (en) 2015-12-16
CA2812991A1 (en) 2012-04-26
BR112013009589A2 (en) 2016-07-19
MX2013004435A (en) 2013-07-29
EA201390583A1 (en) 2013-09-30
JP5977750B2 (en) 2016-08-24
JP2013540152A (en) 2013-10-31
WO2012054029A1 (en) 2012-04-26
WO2012054243A3 (en) 2012-08-02
CA2812991C (en) 2018-09-18

Similar Documents

Publication Publication Date Title
CN103179943B (en) Hair maintenance compositions and correlation technique
CN104095792B (en) Nourishing hair and injury repairing hair conditioner
CN100475178C (en) Stable aqueous surfactant compositions
CN108391418A (en) Include the shampoo Compositions of at least one oligomeric ester ammonium salt
CN101039654B (en) Hair care formulations comprising aminofunctional polyoganosiloxane
JP4977022B2 (en) Hair care composition comprising a dendritic polymer
CN105793273A (en) Dihydroxyalkyl substituted polygalactomannan, and methods for producing and using the same
CN106265109A (en) Strong composition and the strong method sent out and make hair have splendid feel
JP2002516831A (en) Hair treatment composition
JP2002505258A (en) Shampoo composition
AU2003239331B2 (en) Durable hair treatment composition
US20150313832A1 (en) Method of reducing frizz and improving moisturization
CN102958504A (en) Hair care composition
CN102018636A (en) Usage of drying oil for wash-protecting the color of artificially dyed keratin fibers
CN105209000A (en) Process for one-step colouring and straightening hair
US20230355496A1 (en) Concentrate for keratin fiber treatment compositions
RU2213555C2 (en) Composition for taking care for hair
CN1315456C (en) Polysiloxane compositions
CN104168875A (en) Cosmetic composition comprising at least one particular amphoteric polymer and at least one particular conditioning agent
JP5517430B2 (en) Hair deformation second agent, hair deformation agent, and hair deformation treatment method
US10993898B2 (en) Fatty acid esters of oxalkylated alkylalkylenediamines and salts thereof and compositions for conditioning of hair
JP4795245B2 (en) Hair care composition
US20070148122A1 (en) Hair treating composition
JP5887185B2 (en) Hair cosmetics
WO2023234193A1 (en) Production method for aqueous composition

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant