CN1210133A - Production of chlorinated paraffin - Google Patents
Production of chlorinated paraffin Download PDFInfo
- Publication number
- CN1210133A CN1210133A CN97106069.XA CN97106069A CN1210133A CN 1210133 A CN1210133 A CN 1210133A CN 97106069 A CN97106069 A CN 97106069A CN 1210133 A CN1210133 A CN 1210133A
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- CN
- China
- Prior art keywords
- clorafin
- tetracol phenixin
- chlorine
- paraffin
- technology according
- 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.)
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Abstract
A process for preparing chlorowax No.70 uses CCl4 as solvent and includes such steps as photochlorination reaction to obtain mixed liquid of chlorowax No.70 and removing hydrochloric acid and CCl4. It features that CCl4 and H2O are removed by distilling while reducing the pressure. Its raw materials are paraffine and chlorine gas (or liquefied chlorine). Its advantages are simple process, low consumption of energy and low cost.
Description
The invention belongs to the preparation method of industrial chemicals, particularly 70
#The production method of clorafin.
70
#Clorafin, cl content is commonly referred to as 70 at 68～72% clorafin
#Clorafin, outward appearance are white powder, and the water of getting along well at normal temperatures, oxygenant, dilute alkaline soln react; Tasteless nontoxic, as flame-retardant additive, it and antimonous oxide can form polyolefin resin, vibrin, Resins, epoxy, urethane.Natural rubber, synthetic rubber all available it as flame-retardant additive, can be used as the wear preventive additive of lubricating oil in addition; The tackiness agent modification is improved quality of textile products; Applying glue of the mothproof and paper industry of the preservation of timber against decay etc.
Existing 70
#The production technique of clorafin is to be solvent with the tetracol phenixin, chlorine and 42
#Clorafin is a raw material, carries out optical chlorinating reaction under the effect of light, 50～75 ℃ of temperature of reaction, tetracol phenixin and 42
#The weight ratio of clorafin is 3～4: 1, obtain after the reaction 70
#The clorafin mixed solution is washed, is neutralized with alkali lye, and layering separates, and removes wherein hydrochloric acid and chlorine, remaining 70
#The carbon tetrachloride solution of clorafin removes tetracol phenixin and portion water through the normal pressure distillation of heating, after carry out drying, pulverize and obtain water content at Powdered 70 below 1%
#Clorafin.The deficiency that this technology exists is: 70
#During the distillation of the carbon tetrachloride solution of clorafin prior to 65～75 ℃ down through 2-3 hour, temperature raising to 100 ℃ reached 70 of water content 10% through 60 minutes then
#Clorafin.And 70
#It is to make water content below 1% that the technical target of the product of clorafin requires, so must be through super-dry.Need control low temperature when dry, energy consumption is big, and investment is big.If continue to heat up when distillation, product can become color, influences quality product.In addition with 42
#Clorafin is a raw material, or builds 1
#The clorafin workshop increases investment, or buys finished product 42
#Clorafin increases product cost.
The objective of the invention is to improve 70
#The production technique of clorafin cuts down the consumption of energy, investment and cost.
Of the present invention 70
#The production technique of clorafin is a solvent with the tetracol phenixin still, obtains 70 by optical chlorinating reaction
#The mixed solution of clorafin obtains 70 through the purifying treatment of demineralizing acid, tetracol phenixin etc. respectively
#Clorafin, the major technique characteristics are 70
#The carbon tetrachloride solution of clorafin is removed tetracol phenixin and remaining moisture by underpressure distillation.
The underpressure distillation suitable condition is at 0.5～0.8 standard atmospheric pressure, and best 0.6 normal atmosphere carries out under 75～85 ℃.
By underpressure distillation, temperature does not only influence the outward appearance and the quality of product below 100 ℃, and makes water content in the product below 1%, meets the use technology requirement of product.Therefore do not need to reinvest drying plant, thereby reduce energy consumption and production costs.
70
#The raw materials for production of clorafin can be still with chlorine and 42
#Clorafin is a raw material.With the tetracol phenixin is solvent, carries out optical chlorinating reaction under the effect of light, 50～75 ℃ of temperature of reaction, tetracol phenixin and 42
#The weight ratio of clorafin is 3～4: 1, obtain after the reaction 70
#The clorafin mixed solution, the alkali lye neutralizing acid is used in washing, and layering separates, and removes the saline solution of chlorine and generation, remaining 70
#The carbon tetrachloride solution of clorafin carries out underpressure distillation.
70
#The raw materials for production of clorafin can be solvent with the tetracol phenixin with chlorine or liquid chlorine and paraffin, carry out optical chlorinating reaction under 65～75 ℃, and a step generates 70
#Clorafin.The weight ratio of tetracol phenixin and paraffin is 3～4: 1, this moment obtain 70
#The mixed solution of clorafin through washing, is used the alkali lye neutralizing acid, and layering separates again, sloughs the saline solution of generation, remaining 70
#The carbon tetrachloride solution of clorafin carries out underpressure distillation again.After moisture taken off, get and after the sample analysis touches the mark product is emitted, become solid at normal temperatures, be crushed to certain particle diameter.
Advantage of the present invention: removed 70 by underpressure distillation
#Moisture in the clorafin has omitted the operation of oven drying at low temperature, and energy consumption and investment reduce; Be raw material directly, reduced cost with paraffin, liquid chlorine.Its technical indicator is as follows:
| Project | Index request |
| Cl content % | ????68～72 |
| Softening temperature ℃ 〉= | ????95 |
| Granularity | By 100 orders |
| Moisture %≤ | ????1 |
| Heat stability index %≤ | ????0.3 |
Embodiment:
800 kilograms of paraffin enter 5000 liters of reactors, be warmed up to 60 ℃, after treating that paraffin dissolves, drop into liquid chlorine gradually, liquid chlorine adds 2400 kilograms in tetracol phenixin after being metered into 1600 kilograms by under meter, multiple sets of light sources (muriate mercury lamp) is set in the reactor, and temperature is controlled at 65～75 ℃ under the normal pressure, continues introduce chlorine gas to make reaction, after advancing 1800 kilograms of chlorine, observe by visor, constantly put sample and chemically examine every index, the back that touches the mark neutralizes with soda ash solution, with the PH test paper measure be not acidity after, standing demix is isolated the saline solution after the neutralization, 70
#The carbon tetrachloride solution of clorafin enters reactor and carries out underpressure distillation, and pressure is 0.6 standard atmospheric pressure, and 75～85 ℃ of temperature made 70 after 8 hours
#The water content of clorafin is below 1%, and the tetracol phenixin that distills out reclaims through condensation, emits 70 from reactor
#Clorafin becomes solid at normal temperatures, pulverizes, and makes it all to pack by 100 orders, obtains 70
#Clorafin 2000kg.
Among this embodiment, tetracol phenixin is to add after reaction for some time at liquid chlorine and paraffin, has just begun step of reaction and can not need add tetracol phenixin.Tetracol phenixin also can dissolve afterreaction at paraffin to begin once to add.
Claims (6)
1,70
#The production technique of clorafin is a solvent with the tetracol phenixin, obtains 70 by optical chlorinating reaction
#The mixed solution of clorafin obtains 70 through the purifying treatment of demineralizing acid, tetracol phenixin etc. respectively
#Clorafin is characterized in that 70
#The carbon tetrachloride solution of clorafin is removed tetracol phenixin and moisture through underpressure distillation.
2, technology according to claim 1 is characterised in that described underpressure distillation is at 0.5～0.8 standard atmospheric pressure, carries out under 75～85 ℃.
3, technology according to claim 1 is characterised in that 70
#Clorafin is with chlorine and 42
#Clorafin is a raw material.
4, technology according to claim 1 is characterised in that 70
#Clorafin is to be raw material with chlorine or liquid chlorine and paraffin.
5, technology according to claim 4 is characterised in that chlorine or liquid chlorine, paraffin are solvent with the tetracol phenixin, carry out optical chlorinating reaction under 65～75 ℃.
6, technology according to claim 5, the weight ratio that is characterised in that tetracol phenixin and paraffin is 3～4: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106069.XA CN1210133A (en) | 1997-08-29 | 1997-08-29 | Production of chlorinated paraffin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97106069.XA CN1210133A (en) | 1997-08-29 | 1997-08-29 | Production of chlorinated paraffin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1210133A true CN1210133A (en) | 1999-03-10 |
Family
ID=5168345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97106069.XA Pending CN1210133A (en) | 1997-08-29 | 1997-08-29 | Production of chlorinated paraffin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1210133A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8366593B2 (en) | 2008-01-12 | 2013-02-05 | Trumpf Werkzeugmaschinen Gmbh + Co. Kg | Laser nozzle changing device |
| CN103627437A (en) * | 2013-12-20 | 2014-03-12 | 哈尔滨理工大学 | Method for preparing chlorinated paraffin |
| CN106190305A (en) * | 2016-08-03 | 2016-12-07 | 安徽中缘新材料科技有限公司 | A kind of production method of environment friendly chlorinated paraffin 70 |
-
1997
- 1997-08-29 CN CN97106069.XA patent/CN1210133A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8366593B2 (en) | 2008-01-12 | 2013-02-05 | Trumpf Werkzeugmaschinen Gmbh + Co. Kg | Laser nozzle changing device |
| CN103627437A (en) * | 2013-12-20 | 2014-03-12 | 哈尔滨理工大学 | Method for preparing chlorinated paraffin |
| CN103627437B (en) * | 2013-12-20 | 2015-04-15 | 哈尔滨理工大学 | Method for preparing chlorinated paraffin |
| CN106190305A (en) * | 2016-08-03 | 2016-12-07 | 安徽中缘新材料科技有限公司 | A kind of production method of environment friendly chlorinated paraffin 70 |
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Legal Events
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |