EP0698076A1 - Method and plant for solvent-free microwave extraction of natural products - Google Patents
Method and plant for solvent-free microwave extraction of natural productsInfo
- Publication number
- EP0698076A1 EP0698076A1 EP94915607A EP94915607A EP0698076A1 EP 0698076 A1 EP0698076 A1 EP 0698076A1 EP 94915607 A EP94915607 A EP 94915607A EP 94915607 A EP94915607 A EP 94915607A EP 0698076 A1 EP0698076 A1 EP 0698076A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- enclosure
- biological material
- microwaves
- natural product
- extract
- 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
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Definitions
- the invention relates to the field of extraction of natural products contained in biological material and in particular, but not exclusively, the extraction of such products from plants.
- the extraction of natural products from biological material can be carried out according to several processes using or not using one or more extraction solvents, depending on the nature of the biological material used and that of the product or products which it is desired to extract. of it. It should be noted in this regard that the name given to an extract is often a function of the technology used to achieve it.
- the concretes, the resinoids, the oleoresins ... which are extracts consisting of volatile compounds or waxy and fatty and non-volatile products, are conventionally obtained in the presence of at least one organic solvent.
- Essential oils mainly consisting of odorous volatile compounds, are generally obtained by distillation with water vapor (hydrodistillation) and / or by mechanical processes.
- oilseeds, essential oils of citrus peel, fish oils ... is conventionally carried out using physical processes such as grinding and / or pressing, by absence of solvent or by hydrodistillation.
- such techniques have the advantage of making it possible to obtain extraction products (and biological material after extraction) free from solvent residues and therefore having no not undergo subsequent treatment for the removal of such residues.
- extraction techniques using organic solvents. Thanks to such techniques the product to be extracted diffuses into the solvent and dissolves there. However, it is then necessary to separate the extracted product from the solvent, in order to allow the concentration of the extract.
- Many parameters are involved in the extraction yields carried out in the presence of solvent, among which may be mentioned: - the solubility of the product extracted in the chosen solvent,
- the diffusion of the extracted product could be greatly improved by subjecting the biological material to a pretreatment which may consist in particular of grinding, enzymatic digestion or even drying.
- a pretreatment which may consist in particular of grinding, enzymatic digestion or even drying.
- sonication methods which consist in applying ultrasound to the mixture constituted by the biological material and the solvent in order to promote the passage of the extract into the solvent.
- the mechanical waves formed by the ultrasounds indeed make it possible to locally generate a cavitation of the biological material and consequently a heating of the latter promoting the release of the extract.
- European patent EP 0398798 discloses a technique for extracting products from biological material assisted by microwaves, comprising the following steps consisting in: subdivide a biological material (peppermint, Scottish lovage, cedar or garlic) having a dispersed component absorbing microwaves (water), put this subdivided material in a transparent or partially transparent solvent in microwaves and absorbing less micro -waves as the dispersed component, such as hexane, ethanol or dichloromethane, exposing the mixture constituted by the subdivided material and the solvent to the microwaves in order to allow the extraction of the soluble products by heating the subdivided material preferentially with solvent, - separate the residual biological material from the solvent and recover the extracted product.
- subdivide a biological material peppermint, Scottish lovage, cedar or garlic
- a dispersed component absorbing microwaves (water)
- a transparent or partially transparent solvent in microwaves and absorbing less micro -waves as the dispersed component, such as hexan
- the objective of the present invention is to provide a process for extracting natural products by microwave, without having the drawbacks of the processes of the prior art.
- one of the objectives of the invention is to provide such a process allowing extraction in the absence of solvent and therefore obtaining an extract free from any solvent residue.
- Another objective of the invention is to propose such a process without requiring an excessive energy supply, for a given quantity of biological material to be treated.
- Another objective of the invention is to propose an installation for the implementation of such a method.
- the invention relates to a process for the microwave extraction of at least one natural product from biological material, said process consisting in: placing said biological material in an enclosure, in the absence of any solvent, - subjecting said biological material present in said enclosure to microwave irradiation, in order to cause the evaporation of at least part of the water contained in said biological material and consequently the bursting of the cellular structures of said biological material.
- said method being characterized in that it comprises the following additional steps consisting in: applying, intermittently, a reduced pressure inside said enclosure during said step of applying microwaves, in order to promote bursting cellular structures of said biological material induced by the application of microwaves, heating, during at least most of said step of applying microwaves, said enclosure, in order to compensate for the drop in temperature resulting from evaporation water from biological material, the combination of said steps of applying microwaves, applying reduced pressure inside the enclosure and heating the enclosure allowing the hydrodistillation of said natural product by entraining it in water vapor from said biological material.
- Such a process can be advantageously implemented on all natural biological materials, whether they are of animal, plant or micro ⁇ biological origin as long as these contain at least about 30% water.
- This process can in particular be used to extract essential oils from plants, tissues of animal origin and especially from fish, but also from algae, micro-algae and even possibly micro-organisms.
- this biological material may, depending on its nature, be subdivided before being introduced into the enclosure in order to increase its factor of exposure to microwaves.
- the process according to the invention makes it possible to carry out the hydrodistillation of the product which it is desired to extract, not thanks to water brought from outside during the process, but thanks to the water contained in the biological material. treaty.
- this water will be called water of constitution, whereas it may have been brought beforehand to the biological material, when the latter will be available in dehydrated form, during a rehumidification stage.
- the method according to the invention therefore consists in subjecting the treated biological material to microwave radiation, in the absence of extracting solvent, allowing the contents of the cells of this material to be ejected outside.
- the pressure of the enclosure is reduced. This reduction in pressure makes it possible, on the one hand, to increase the mechanical stress exerted on the walls of the cells of the biological material and on the other hand to increase the volatility of the azeotropic mixture constituted by the product which it is desired to extract and water vapor.
- the concomitant heating of the enclosure makes it possible to compensate for the very rapid decrease in temperature resulting from the evaporation of the water of constitution under the effect of the lowering of the pressure in the enclosure.
- Such a decrease in temperature is indeed capable of completely masking the action of microwaves.
- the method according to the invention has many advantages. In addition to the fact that it leads to extracts without residual solvent, it also makes it possible, with respect to a conventional hydrodistillation, to obtain an extract of equivalent composition and with an equivalent yield, in a substantially shorter time. While the conventional hydrodistillation times are generally counted in hours, the hydrodistillation times under reduced pressure according to the invention are counted in minutes. For certain products, it is thus possible to obtain a given quantity of extract ten times faster than with a conventional steam distillation.
- the method according to the invention consumes much less energy than the microwave assisted extraction methods of the prior art.
- the energy used in the context of the invention is also less than that necessary for hydrodistillation.
- hydrodistillation it is indeed necessary to heat the biological material and the added water, the mass of which can represent up to 10 times the mass of biological material.
- the residual biological material obtained at the end of the process is in a dry form, since the water of constitution which it contained was used for the entrainment of the extracted product and that the process does not put using external water supply. Consequently, this residual material can easily be degraded thermally and therefore possibly recycled as fuel.
- said step of the method according to the invention consisting of the intermittent application of a reduced pressure, consists in subjecting the interior of said enclosure to vacuum cycles.
- said step of separation of the residual biological material from the extract consists:
- said heating step is preferably carried out at a temperature below 100 ° C.
- the process can be carried out at a temperature advantageously below 75 ° C so as to allow the extraction of products which tend to degrade under the effect of heat.
- the microwaves used during said microwave irradiation step advantageously have a frequency at least equal to 300 MHz. It should be noted, however, that in many countries the use of frequencies is very strictly regulated and that, for example in France, only frequencies of 915 MHz and
- said microwave irradiation step will preferably be carried out so as to apply a power ranging from approximately 100 W to approximately 10,000 W per kilogram of product treated.
- said microwave irradiation step is carried out with mechanical stirring of said biological material. Such agitation will increase the factor of exposure of biological material to microwaves.
- the invention also relates to an installation for implementing such a method, characterized in that it comprises:
- Means for recovering the extract at its exit from said enclosure comprise means for refrigerating the water vapor containing the extract.
- said installation has means for operating said means making it possible to reduce the pressure inside the enclosure cyclically.
- said enclosure is provided with stirring means.
- said installation comprises means making it possible to redirect the waste water obtained at the level of the means for recovering the extract inside said enclosure.
- FIG. 1 shows a schematic view of an installation according to the invention
- FIG. 2 translates the evolution of the pressure of the enclosure and the temperature of the biological material, in the context of a first example of implementation of the method according to the invention with the installation shown schematically in Figure 1 , for the extraction of peppermint essential oil;
- FIG. 4 shows the evolution of the pressure of the enclosure and the temperature of the biological material, in the context of a comparative example of extraction of peppermint essential oil
- FIG. 6 shows the evolution of the pressure of the enclosure and the temperature of the biological material, in the context of a second example of implementation of the method according to the invention for the extraction of essential oil from officinal sage;
- FIG. 7 shows the evolution of the essential oil yield of sage sage obtained during the second example of implementation of the method according to the invention.
- an installation for extracting natural products from biological material is shown schematically.
- Such an installation comprises an enclosure 1 equipped with means 2 making it possible to generate microwaves in the interior volume which it delimits.
- these means 2 allow the emission of microwaves having a frequency equal to 2450 MHz. (Note that it would also have been possible to use a microwave generator with a frequency of 915 MHz, this other frequency being also authorized in France).
- the enclosure 1 is also provided in its lower part with stirring means 9, constituted by a turbine with three blades, making it possible to stir the biological material during its presence inside the enclosure 1, when subjected to the action of microwaves.
- stirring means 9 constituted by a turbine with three blades, making it possible to stir the biological material during its presence inside the enclosure 1, when subjected to the action of microwaves.
- Such stirring makes it possible to increase the exposure of the biological material to microwaves and to prevent certain areas of the latter from being insufficiently irradiated to carry out the extraction operation.
- the enclosure 1 is connected on the one hand with means 5 making it possible to reduce the pressure prevailing therein and, on the other hand, with means 6 for recovering the natural product extracted thanks to the action of microwaves on biological material.
- the means 5 making it possible to reduce the pressure in the enclosure can consist of any means conventionally used for the purpose of creating a partial vacuum inside an enclosure, such as, for example, a pump or a suction tube. water.
- the means 6 for recovering the extracted product comprise a pipe 11 installed in the upper part of the enclosure 1, around which are provided cooling means 7 formed by a coil in which a liquid circulates. cooling.
- Line 11 makes it possible to recover the vapors resulting from the action of microwaves on biological material and in which the essential oil is found. Thanks to the refrigeration means 7 these water vapors are condensed.
- a decanter 12 is provided at the outlet of the pipe 11 to recover these condensed vapors and separate the essential oil. The remaining waste water, after decantation is advantageously re-routed, through a pipe 10 in the enclosure 1 where it is recycled to complete the extraction.
- the enclosure 1 In order to allow heating of the interior of the enclosure 1 to compensate for the decrease in temperature resulting from the lowering of the pressure induced by the vacuum pump 5, the enclosure 1 has a thermostated double wall 3 connected to heating means 4.
- a kilogram of peppermint (Mentha piperita L., Hungarian variety) with 15% dry matter was placed inside the enclosure 1.
- the heating means 4 were adjusted so that the thermostatically controlled wall 3 induce a temperature of about 70 ° C inside the enclosure 1 and the stirring means 9 have been implemented so as to have a speed of 40 revolutions per minute.
- the power emitted by the microwave generation means 2 is 1150 W and the reflected power varies between 170 W and 220 W. During the extraction operation, which lasted 15 min, the power actually absorbed therefore been from 930 to 980 W.
- the pump 5 was implemented so as to lower the pressure to 250 mb. This pressure reduction was carried out after 5 min, 10 min and 13 min.
- the temperature of the refrigeration medium circulating in the coil 7 was fixed at 5 ° C. so as to cause the condensation of the vapors resulting from the action of the microwaves on the peppermint and containing the essential oil.
- the evolution of the temperature of the mint present in the enclosure and of the pressure prevailing inside it is represented in FIG. 2.
- the temperature of the product rapidly changes from room temperature up to about 75 ° C.
- the temperature drops. This drop in temperature is quickly compensated for by heating the enclosure so as not to mask the action of the microwaves.
- Example 1 The same quantity of peppermint as in Example 1 was treated using the same operating conditions as in Example 1 but by continuously operating the pump 5 so that the pressure prevailing inside the enclosure 1 is fixed at 250 mb during the entire extraction operation.
- Example 3 The change in the temperature of the mint and the pressure in the enclosure is given in FIG. 4. With reference to FIG. 5, the yield of essential oil was then only 0.2 ml per 100 g, or 5 times less than in Example 1. 1150 mg of essential oil were recovered from the mint residue after the extraction operation. These results show the importance of the intermittent nature which must be given, according to the invention, to the lowering of the pressure inside the enclosure.
- the heating means 4 have been adjusted so that the thermostatically controlled wall 3 induces a temperature of around 70 ° C. inside the enclosure 1 and the stirring means 9 have been implemented so as to have a speed of 40 revolutions per minute.
- the power emitted by the microwave generation means 2 is 1000 W and the reflected power varies between 150 W and 200 W. During the extraction operation, which lasted 10 min, the power actually absorbed therefore was from 800 to 850 W. During the extraction, the pump 5 was implemented so as to reduce the pressure to 250 mb. This pressure reduction was carried out after 3.5 min and 7 min.
- the temperature of the refrigeration medium circulating in the coil 7 was fixed at 5 ° C. so as to cause the condensation of the vapors resulting from the action of the microwaves on the peppermint and containing the oil. essential.
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR9305810A FR2705035B1 (en) | 1993-05-11 | 1993-05-11 | Process and installation for solvent-free extraction of natural products by microwave. |
FR9305810 | 1993-05-11 | ||
PCT/FR1994/000551 WO1994026853A1 (en) | 1993-05-11 | 1994-05-10 | Method and plant for solvent-free microwave extraction of natural products |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0698076A1 true EP0698076A1 (en) | 1996-02-28 |
EP0698076B1 EP0698076B1 (en) | 1998-01-14 |
Family
ID=9447117
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP94915607A Expired - Lifetime EP0698076B1 (en) | 1993-05-11 | 1994-05-10 | Method and plant for solvent-free microwave extraction of natural products |
Country Status (16)
Country | Link |
---|---|
EP (1) | EP0698076B1 (en) |
JP (1) | JPH08512337A (en) |
CN (1) | CN1059920C (en) |
AT (1) | ATE162211T1 (en) |
AU (1) | AU682035B2 (en) |
BG (1) | BG62367B1 (en) |
BR (1) | BR9406717A (en) |
CA (1) | CA2161127C (en) |
DE (1) | DE69407965T2 (en) |
DK (1) | DK0698076T3 (en) |
ES (1) | ES2114688T3 (en) |
FR (1) | FR2705035B1 (en) |
GR (1) | GR3026603T3 (en) |
HU (1) | HU218708B (en) |
RU (1) | RU2115700C1 (en) |
WO (1) | WO1994026853A1 (en) |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1439218A1 (en) * | 2003-01-21 | 2004-07-21 | Milestone S.r.l. | Solvent-free microwave extraction of volatile natural compounds |
FR2955331A1 (en) * | 2010-01-15 | 2011-07-22 | Archimex Pibs | Extracting natural product comprising volatile molecule from biological material by microwaves, comprises placing biological material in enclosure, extracting volatile natural product from biological material, and heating the enclosure |
WO2012056141A2 (en) | 2010-10-29 | 2012-05-03 | Bernard Mompon | Method for producing articles of plant origin impregnated with a liquid plant substance |
WO2012156361A1 (en) | 2011-05-13 | 2012-11-22 | Universite D'avignon Et Des Pays De Vaucluse | Preparation of a plant extract using microwaves |
FR3003181A1 (en) * | 2013-03-18 | 2014-09-19 | Innovation & Dev Company Idco | METHOD AND INSTALLATION FOR EXTRACTING BIOLOGICAL PRODUCTS BY MICROWAVES |
FR3017309A1 (en) | 2014-02-10 | 2015-08-14 | Idco | PROCESS FOR EXTRACTING BIOLOGICAL PRODUCTS BY RECYCLING MICROWAVE ASSISTED THIN FILM SOLVENT |
CN106190574A (en) * | 2016-07-28 | 2016-12-07 | 河南科技学院 | A kind of Atractylodes lancea (Thunb.) DC. volatile oil and preparation method thereof |
WO2019106313A1 (en) | 2017-12-01 | 2019-06-06 | Université D'avignon Et Des Pays De Vaucluse | Device for extracting and separating volatile and non-volatile compounds from a biological material, and associated process |
FR3099991A1 (en) | 2019-08-22 | 2021-02-26 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Cosmetic composition ingredient for sensitive scalp |
FR3113248A1 (en) | 2020-08-04 | 2022-02-11 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Lavandula stoechas cell extract, compositions comprising it, cosmetic uses and method for culturing Lavandula stoechas cells. |
FR3115695A1 (en) | 2020-10-30 | 2022-05-06 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Active ingredient consisting of a bitter apple extract activating Tas2Rs bitterness receptors present on human skin and corresponding cosmetic and dermato-cosmetic uses. |
Families Citing this family (52)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2763795B1 (en) * | 1997-05-30 | 1999-08-20 | Archimex Pibs | PROCESS FOR THE PREPARATION OF PLANTS SUCH AS SPICES, AROMATIC PLANTS AND AROMATOES |
FR2793008B1 (en) | 1999-04-30 | 2001-07-27 | Valeurs Bois Ind | PROCESS FOR THE EXTRACTION OF NATURAL JUICE FROM WOODY PLANT MATERIAL, DEVICE FOR CARRYING OUT THE PROCESS AND USE OF THE PROCESS FOR THE PRODUCTION OF DRY WOODY PLANT |
FR2787347B1 (en) * | 1998-12-17 | 2001-01-19 | Gattefosse Ets Sa | METHOD FOR MANUFACTURING AN EMULSION BASED ON AROMATIC PLANT MATERIAL, EMULSION LIKELY TO BE OBTAINED BY SAID METHOD AND USE OF SAID EMULSION |
CN1112953C (en) * | 1999-10-29 | 2003-07-02 | 汤大卫 | Process for liquid/sodid extraction |
CN1120736C (en) * | 2000-09-14 | 2003-09-10 | 中国科学院山西煤炭化学研究所 | Extraction process for industrial solid material |
DE502004008822D1 (en) * | 2004-07-20 | 2009-02-26 | Milestone Srl | Microwave assisted extraction of volatile natural products |
CN100379754C (en) * | 2004-11-22 | 2008-04-09 | 王煊 | Extraction of saponin by non-solvent microwave heat |
CN100421759C (en) * | 2006-03-10 | 2008-10-01 | 山东轻工业学院 | Decompressed microwave extraction device and method for extracting plant effective ingredient |
EP2011568B1 (en) * | 2006-03-16 | 2016-08-24 | Universidad Tecnica Federico Santa Maria (Usm) | Device for extraction of organic chemical compounds with toxic properties that are present in atmospheric samples, using focused-microwave-heated solvents in open (non-pressurized) systems |
CN101290277B (en) * | 2007-04-20 | 2011-05-11 | 财团法人食品工业发展研究所 | Rapid extraction method utilizing microwave radiation |
TW200842336A (en) * | 2007-04-26 | 2008-11-01 | Food Industry Res & Dev Inst | Microwave accelerating extraction equipment |
FR2925898A1 (en) * | 2007-12-28 | 2009-07-03 | Jean Pierre Lablanchy | Extracting an essential oil having high content of thymoquinone from a part of Nigella sativa plant, comprises extracting aromatic water comprising essential oil using combination of microwave and impulse vacuum |
JP5508388B2 (en) * | 2009-02-26 | 2014-05-28 | エステー株式会社 | High monoterpene component-containing essential oil, method for producing the same, and method for purifying environmental pollutants using the essential oil |
RU2395766C1 (en) * | 2009-05-25 | 2010-07-27 | Закрытое Акционерное Общество "Твин Трейдинг Компани" | Drying method of materials of vegetable, animal origin, fish and seafood, and device for its implementation |
JP2011052086A (en) * | 2009-08-31 | 2011-03-17 | Actree Corp | Method for extracting oil and fat from bryophyte |
JP6087485B2 (en) * | 2010-02-25 | 2017-03-01 | エステー株式会社 | Fragrance composition and fragrance, deodorant and antibacterial agent using the same |
TWI468506B (en) * | 2011-01-17 | 2015-01-11 | Nat Univ Chung Hsing | The method and application of microwave-assisted extraction for microalgae lipid |
CN102252889A (en) * | 2011-03-15 | 2011-11-23 | 重庆大学 | Microwave-assisted solvent-free solid-phase headspace extraction device and extraction method thereof |
LV14481B (en) * | 2011-11-21 | 2012-06-20 | Latvijas Valsts Mežzinātnes Institūts 'silava' | Method of production of water soluble and non-soluble essential oils from plant origin raw material |
RU2473356C1 (en) * | 2011-12-07 | 2013-01-27 | Общество с ограниченной ответственностью "Компания Клевер" | Method for preparing aqueous extracts of crude drugs rich in active extractants |
US9486716B2 (en) | 2012-03-14 | 2016-11-08 | State Of Oregon Acting By And Through The State Board Of Higher Education On Behalf Of Oregon State University | Essential oil extraction apparatus |
CN103194312A (en) * | 2013-03-24 | 2013-07-10 | 西北农林科技大学 | Method for extracting essential oil from cypress leaves |
FR3013563B1 (en) * | 2013-11-28 | 2017-06-30 | Finat Conseil & Distrib | PROCESS FOR MANUFACTURING NATURAL AND STABLE AROMATIZING PREPARATIONS AND AROMATIZING PREPARATIONS OBTAINED BY SAID METHOD |
CN103725420B (en) * | 2013-12-20 | 2016-07-13 | 江南大学 | A kind of extract the method for Nigella damascena L. platymiscium Volatile Oil from Seed, device and application |
CN103820218A (en) * | 2014-03-07 | 2014-05-28 | 张家界金绿油脂有限责任公司 | Method for microwave extracting rapeseed grease |
JP5899604B2 (en) * | 2014-03-24 | 2016-04-06 | 兼松エンジニアリング株式会社 | Biomass recycling system using microwaves |
TWI601565B (en) * | 2014-06-05 | 2017-10-11 | Timing Pharmaceutical Co Ltd | Essential oil extraction device |
CN104327951A (en) * | 2014-10-23 | 2015-02-04 | 郑州工业应用技术学院 | Hot air essential oil extraction device |
CN104872605B (en) * | 2014-12-08 | 2018-02-06 | 中国热带农业科学院南亚热带作物研究所 | The method and liquid fumet of preparation solution fumet |
RO130896A0 (en) * | 2015-01-19 | 2016-02-26 | Mariana Pătraşcu | Continuous flow reactor for microwave- and ultrasound-assisted extraction of biologically active compounds from plants |
CN104711121A (en) * | 2015-02-28 | 2015-06-17 | 湖北中烟工业有限责任公司 | Method for extracting chrysanthemum indicum essential oil in ultrasonic-assisted solvent-free microwave extraction manner |
CN104784965B (en) * | 2015-04-20 | 2016-10-05 | 张新泉 | A kind of microwave extracting device for Chinese medicine |
RU2582292C1 (en) * | 2015-05-07 | 2016-04-20 | федеральное государственное автономное образовательное учреждение высшего образования "Российский университет дружбы народов" (РУДН) | Method of extracting essential oil from medicinal plant material |
CN105219526A (en) * | 2015-09-25 | 2016-01-06 | 四川省林业科学研究院 | A kind of yusho oil microwave extraction device and method |
CN105213272B (en) * | 2015-11-09 | 2019-02-01 | 北京工商大学 | A kind of fresh and alive water of lavender and the preparation method and application thereof |
CN105232400B (en) * | 2015-11-09 | 2018-11-02 | 北京工商大学 | A kind of fresh and alive water of jasmine and the preparation method and application thereof |
CN105250180B (en) * | 2015-11-09 | 2018-11-27 | 北京工商大学 | A kind of fresh and alive water of rose and the preparation method and application thereof |
CN105232782B (en) * | 2015-11-09 | 2019-11-22 | 北京工商大学 | A kind of fresh and alive water of fresh tea and the preparation method and application thereof |
CN105213273B (en) * | 2015-11-09 | 2018-11-13 | 北京工商大学 | A kind of fresh and alive water of lemon and the preparation method and application thereof |
CN105713726A (en) * | 2016-03-31 | 2016-06-29 | 李颖 | Method and device for rapidly extracting natural plant essential oil and hydrolat without solvents |
JP2017008111A (en) * | 2016-10-17 | 2017-01-12 | エステー株式会社 | Aromatic composition and aromatic agent using the same, deodorant and antibacterial agent |
RU2636155C1 (en) * | 2016-12-20 | 2017-11-21 | Федеральное Государственное Бюджетное Образовательное Учреждение Высшего Образования "Нижегородская Государственная Сельскохозяйственная Академия" (ФГБОУ ВО НГСХА) | Microwave technology for extracting fat from fat-containing raw materials |
RU2649024C1 (en) * | 2017-01-10 | 2018-03-29 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кубанский государственный технологический университет" (ФГБОУ ВО "КубГТУ") | Method for obtaining the essential peppermint oil |
FR3066703B1 (en) * | 2017-05-24 | 2020-10-16 | Erpim | SOLID / LIQUID BACK-CURRENT EXTRACTION PROCESS AND DEVICE INCLUDING A DRYING STAGE |
BR112020003196A2 (en) * | 2017-08-31 | 2020-09-29 | Firmenich S.A. | microwave-assisted extraction of essential oils from plant biomass |
JP6359752B1 (en) * | 2017-12-22 | 2018-07-18 | 日本フレーバー工業株式会社 | Manufacturing method of vanilla extract and vanilla extract |
CN110747060A (en) * | 2019-10-21 | 2020-02-04 | 华侨大学 | Method for extracting melaleuca alternifolia essential oil by ultrasonic-assisted solvent-free microwave |
WO2022123989A1 (en) * | 2020-12-08 | 2022-06-16 | エステー株式会社 | Excrement treatment material and excrement deodorization method using same |
CN112760166A (en) * | 2021-01-08 | 2021-05-07 | 四川轻化工大学 | Rattan pepper oil production facility |
WO2022163063A1 (en) * | 2021-01-28 | 2022-08-04 | エステー株式会社 | Excrement treatment material and excrement deodorization method using same |
CN113388459B (en) * | 2021-05-26 | 2022-03-01 | 宁波芮颂生物科技有限公司 | Preparation method of anti-cat and dog allergen finishing composition solution |
US11702615B1 (en) | 2022-03-09 | 2023-07-18 | Chemtech Services, Inc. | Microwave extraction of essential oils |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA1336968C (en) * | 1989-05-16 | 1995-09-12 | J. R. Jocelyn Pare | Microwave-assisted natural products extraction |
SE9003593D0 (en) * | 1990-11-12 | 1990-11-12 | T G Owe Berg | PROCEDURE FOR CONVERSION OF HEATS TO WORK |
ES2082822T3 (en) * | 1990-11-16 | 1996-04-01 | United Kingdom Government | MICROWAVE EXTRACTION OF VOLATILE OILS AND APPARATUS FOR THE SAME. |
-
1993
- 1993-05-11 FR FR9305810A patent/FR2705035B1/en not_active Expired - Fee Related
-
1994
- 1994-05-10 JP JP6525060A patent/JPH08512337A/en not_active Ceased
- 1994-05-10 DK DK94915607T patent/DK0698076T3/en active
- 1994-05-10 AU AU67251/94A patent/AU682035B2/en not_active Ceased
- 1994-05-10 AT AT94915607T patent/ATE162211T1/en not_active IP Right Cessation
- 1994-05-10 WO PCT/FR1994/000551 patent/WO1994026853A1/en active IP Right Grant
- 1994-05-10 CA CA002161127A patent/CA2161127C/en not_active Expired - Fee Related
- 1994-05-10 DE DE69407965T patent/DE69407965T2/en not_active Expired - Lifetime
- 1994-05-10 HU HU9503230A patent/HU218708B/en not_active IP Right Cessation
- 1994-05-10 RU RU95122234A patent/RU2115700C1/en active
- 1994-05-10 BR BR9406717A patent/BR9406717A/en not_active IP Right Cessation
- 1994-05-10 EP EP94915607A patent/EP0698076B1/en not_active Expired - Lifetime
- 1994-05-10 CN CN94192507A patent/CN1059920C/en not_active Expired - Fee Related
- 1994-05-10 ES ES94915607T patent/ES2114688T3/en not_active Expired - Lifetime
-
1995
- 1995-12-04 BG BG100187A patent/BG62367B1/en unknown
-
1998
- 1998-04-10 GR GR980400799T patent/GR3026603T3/en unknown
Non-Patent Citations (1)
Title |
---|
See references of WO9426853A1 * |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1439218A1 (en) * | 2003-01-21 | 2004-07-21 | Milestone S.r.l. | Solvent-free microwave extraction of volatile natural compounds |
FR2955331A1 (en) * | 2010-01-15 | 2011-07-22 | Archimex Pibs | Extracting natural product comprising volatile molecule from biological material by microwaves, comprises placing biological material in enclosure, extracting volatile natural product from biological material, and heating the enclosure |
WO2012056141A2 (en) | 2010-10-29 | 2012-05-03 | Bernard Mompon | Method for producing articles of plant origin impregnated with a liquid plant substance |
WO2012156361A1 (en) | 2011-05-13 | 2012-11-22 | Universite D'avignon Et Des Pays De Vaucluse | Preparation of a plant extract using microwaves |
FR3003181A1 (en) * | 2013-03-18 | 2014-09-19 | Innovation & Dev Company Idco | METHOD AND INSTALLATION FOR EXTRACTING BIOLOGICAL PRODUCTS BY MICROWAVES |
FR3017309A1 (en) | 2014-02-10 | 2015-08-14 | Idco | PROCESS FOR EXTRACTING BIOLOGICAL PRODUCTS BY RECYCLING MICROWAVE ASSISTED THIN FILM SOLVENT |
CN106190574A (en) * | 2016-07-28 | 2016-12-07 | 河南科技学院 | A kind of Atractylodes lancea (Thunb.) DC. volatile oil and preparation method thereof |
WO2019106313A1 (en) | 2017-12-01 | 2019-06-06 | Université D'avignon Et Des Pays De Vaucluse | Device for extracting and separating volatile and non-volatile compounds from a biological material, and associated process |
FR3099991A1 (en) | 2019-08-22 | 2021-02-26 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Cosmetic composition ingredient for sensitive scalp |
FR3113248A1 (en) | 2020-08-04 | 2022-02-11 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Lavandula stoechas cell extract, compositions comprising it, cosmetic uses and method for culturing Lavandula stoechas cells. |
FR3115695A1 (en) | 2020-10-30 | 2022-05-06 | Société de Courtage et de Diffusion - CODIF INTERNATIONAL | Active ingredient consisting of a bitter apple extract activating Tas2Rs bitterness receptors present on human skin and corresponding cosmetic and dermato-cosmetic uses. |
Also Published As
Publication number | Publication date |
---|---|
AU6725194A (en) | 1994-12-12 |
HUT75578A (en) | 1997-05-28 |
CA2161127A1 (en) | 1994-11-24 |
ES2114688T3 (en) | 1998-06-01 |
FR2705035A1 (en) | 1994-11-18 |
CA2161127C (en) | 2005-09-27 |
FR2705035B1 (en) | 1995-08-04 |
BR9406717A (en) | 1996-02-06 |
EP0698076B1 (en) | 1998-01-14 |
WO1994026853A1 (en) | 1994-11-24 |
CN1125461A (en) | 1996-06-26 |
DK0698076T3 (en) | 1998-09-14 |
CN1059920C (en) | 2000-12-27 |
HU9503230D0 (en) | 1996-01-29 |
HU218708B (en) | 2000-11-28 |
ATE162211T1 (en) | 1998-01-15 |
BG100187A (en) | 1996-05-31 |
BG62367B1 (en) | 1999-09-30 |
AU682035B2 (en) | 1997-09-18 |
GR3026603T3 (en) | 1998-07-31 |
DE69407965D1 (en) | 1998-02-19 |
RU2115700C1 (en) | 1998-07-20 |
JPH08512337A (en) | 1996-12-24 |
DE69407965T2 (en) | 1998-09-10 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP0698076B1 (en) | Method and plant for solvent-free microwave extraction of natural products | |
US7001629B1 (en) | Method and plant for solvent-free microwave extraction of natural products | |
EP0398798B1 (en) | Extraction of natural products assisted by microwaves | |
EP1261684B1 (en) | Method for fractionating cooking oil | |
EP0238527B1 (en) | Method and device for extracting constituents by means of a supercritical fluid or a pressure liquid | |
FR2817556A1 (en) | PROCESS AND APPARATUS FOR INTEGRAL RECOVERY OF OLEIFIED DRUPS, IN PARTICULAR OLIVES AND THE SPECIFIC PRODUCTS OBTAINED | |
CN1061729A (en) | The extracting process of microwave-assisted and equipment thereof | |
FR3032892A1 (en) | DEVICE AND METHOD FOR ASSISTED EXTRACTION OF PRODUCT ASSETS | |
US5338557A (en) | Microwave extraction of volatile oils | |
FR3003181A1 (en) | METHOD AND INSTALLATION FOR EXTRACTING BIOLOGICAL PRODUCTS BY MICROWAVES | |
FR3074425A1 (en) | DEVICE FOR EXTRACTING AND SEPARATING VOLATILE AND NON-VOLATILE COMPOUNDS FROM BIOLOGICAL MATERIAL AND ASSOCIATED METHOD | |
EP3362078B1 (en) | Novel organic solubilisation and/or extraction solvent, extraction method using said solvent, and extracts obtained by said method | |
FR2973716A1 (en) | PROCESS FOR EXTRACTING AN ODORANT EXTRACT FROM A SOLVENT ALTERNATIVE TO CONVENTIONAL SOLVENTS | |
FR2955331A1 (en) | Extracting natural product comprising volatile molecule from biological material by microwaves, comprises placing biological material in enclosure, extracting volatile natural product from biological material, and heating the enclosure | |
WO1995003380A1 (en) | Process for extracting essential oils from plants through cold maceration and cold deterpenating | |
FR3053340A1 (en) | PROCESS AND INSTALLATION FOR CONTROLLED PARTIAL DEPOLYMERIZATION OF POLYSACCHARIDES | |
FR2717492A1 (en) | Extraction of essential oil from plant material | |
FR2763795A1 (en) | Preservation of aromatic plant material by drying | |
EP4142676A1 (en) | Method for extracting odour from a plant material, in particular from mute flowers, in solid form | |
WO1989000187A1 (en) | Process for extracting essential oils from aromatic plants and products so obtained | |
WO2024002842A1 (en) | System and method for extracting volatile molecules from plant raw materials | |
FR2960000A1 (en) | Reducing amount of furocoumarins in preparation of essential oil, comprises submitting portion of plant containing furocoumarins to microwave radiation, placing obtained extract to fall by gravity out of microwave oven and recovering oil | |
FR3138267A1 (en) | Process for extracting, concentrating and preserving natural truffle aromas without any other excipient on a dry medium | |
IL111684A (en) | Process and installation for extracting products of biological origin without solvents using microwave heating | |
CH270047A (en) | Process for removing water from a product, and device for carrying out this process. |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
17P | Request for examination filed |
Effective date: 19951113 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AT BE CH DE DK ES FR GB GR IE IT LI LU MC NL PT SE |
|
17Q | First examination report despatched |
Effective date: 19960607 |
|
GRAG | Despatch of communication of intention to grant |
Free format text: ORIGINAL CODE: EPIDOS AGRA |
|
GRAG | Despatch of communication of intention to grant |
Free format text: ORIGINAL CODE: EPIDOS AGRA |
|
GRAH | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOS IGRA |
|
GRAH | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOS IGRA |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AT BE CH DE DK ES FR GB GR IE IT LI LU MC NL PT SE |
|
REF | Corresponds to: |
Ref document number: 162211 Country of ref document: AT Date of ref document: 19980115 Kind code of ref document: T |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP |
|
REF | Corresponds to: |
Ref document number: 69407965 Country of ref document: DE Date of ref document: 19980219 |
|
ITF | It: translation for a ep patent filed |
Owner name: PORTA CHECCACCI E BOTTI S.R.L. |
|
GBT | Gb: translation of ep patent filed (gb section 77(6)(a)/1977) |
Effective date: 19980414 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FG2A Ref document number: 2114688 Country of ref document: ES Kind code of ref document: T3 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: FG4D Free format text: 78404 |
|
REG | Reference to a national code |
Ref country code: PT Ref legal event code: SC4A Free format text: AVAILABILITY OF NATIONAL TRANSLATION Effective date: 19980407 |
|
REG | Reference to a national code |
Ref country code: DK Ref legal event code: T3 |
|
PLBE | No opposition filed within time limit |
Free format text: ORIGINAL CODE: 0009261 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT |
|
26N | No opposition filed | ||
REG | Reference to a national code |
Ref country code: GB Ref legal event code: IF02 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: CH Payment date: 20020429 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: IE Payment date: 20020508 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: BE Payment date: 20020517 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: PT Payment date: 20020520 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: GR Payment date: 20020523 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: SE Payment date: 20020524 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: LU Payment date: 20020527 Year of fee payment: 9 Ref country code: DK Payment date: 20020527 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: NL Payment date: 20020528 Year of fee payment: 9 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: MC Payment date: 20020529 Year of fee payment: 9 Ref country code: AT Payment date: 20020529 Year of fee payment: 9 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LU Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030510 Ref country code: AT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030510 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030511 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030512 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: LI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030531 Ref country code: CH Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030531 Ref country code: BE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030531 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: MC Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20030915 |
|
BERE | Be: lapsed |
Owner name: *ARCHIMEX Effective date: 20030531 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: PT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20031130 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: NL Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20031201 Ref country code: DK Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20031201 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: GR Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20031203 |
|
REG | Reference to a national code |
Ref country code: DK Ref legal event code: EBP |
|
EUG | Se: european patent has lapsed | ||
REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
NLV4 | Nl: lapsed or anulled due to non-payment of the annual fee |
Effective date: 20031201 |
|
REG | Reference to a national code |
Ref country code: PT Ref legal event code: MM4A Free format text: LAPSE DUE TO NON-PAYMENT OF FEES Effective date: 20031130 |
|
REG | Reference to a national code |
Ref country code: IE Ref legal event code: MM4A |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: GB Payment date: 20090521 Year of fee payment: 16 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: ES Payment date: 20100520 Year of fee payment: 17 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: TP |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: IT Payment date: 20100519 Year of fee payment: 17 Ref country code: DE Payment date: 20100609 Year of fee payment: 17 |
|
GBPC | Gb: european patent ceased through non-payment of renewal fee |
Effective date: 20100510 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: GB Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20100510 |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R119 Ref document number: 69407965 Country of ref document: DE |
|
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R119 Ref document number: 69407965 Country of ref document: DE |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: IT Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20110510 |
|
REG | Reference to a national code |
Ref country code: ES Ref legal event code: FD2A Effective date: 20120717 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: ES Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20110511 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: DE Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20111130 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: FR Payment date: 20130530 Year of fee payment: 20 |
|
REG | Reference to a national code |
Ref country code: FR Ref legal event code: TP Owner name: SAS AMADEITE, FR Effective date: 20141119 |