CN101157701A - Method for preparing bischloromethyl-tetramethyl disiloxane by hydrolysis of chloromethyl-dimethylchlorosilane - Google Patents
Method for preparing bischloromethyl-tetramethyl disiloxane by hydrolysis of chloromethyl-dimethylchlorosilane Download PDFInfo
- Publication number
- CN101157701A CN101157701A CNA200710156556XA CN200710156556A CN101157701A CN 101157701 A CN101157701 A CN 101157701A CN A200710156556X A CNA200710156556X A CN A200710156556XA CN 200710156556 A CN200710156556 A CN 200710156556A CN 101157701 A CN101157701 A CN 101157701A
- Authority
- CN
- China
- Prior art keywords
- organic layer
- chloromethyl
- dichloromethyl
- hydrolysis
- reaction
- 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.)
- Pending
Links
Abstract
The invention discloses a preparation method of dichloromethyl-tetramethyldisiloxane by the hydrolysis of chloromethyl-dimethyl chlorosilane. The invention takes chloromethyl-dimethyl chlorosilane as the raw materials, which are directly dropped into water for hydrolysis so as to prepare the dichloromethyl-tetramethyldisiloxane, the invention dose not need to be heated and utilizes the heat of the reaction to complete the reaction, the reaction temperature is controlled at 20 to 100 DEG C, an organic layer is separated by cooling down to the room temperature after the completion of dropping, the organic layer is washed by water till neutral, the organic layer is dried, the distillation fractions with a boiling point of 200 to 202 DEG C are collected by distillation, the yield is 95 to 98 percent and the purity is 97 to 99 percent. The invention can overcome the shortcomings of the existing preparation methods of dichloromethyl-tetramethyldisiloxane so as to provide a method which is applicable to the industrial production and has the advantages of high yield, raw material-saving, energy-saving, time-saving, low cost, high efficiency and simple operation.
Description
Technical field
The present invention relates to the method for chemical preparation dichloromethyl-tetramethyl disiloxane, is raw material with chloromethyl-dimethylchlorosilane particularly, and direct hydrolysis prepares the method for dichloromethyl-tetramethyl disiloxane.
Background technology
Organosilicon product has the characteristic of organism and inorganics concurrently, be to have one of novel material of development potentiality most, in electronic apparatus, automobile, building, lightization, chemical industry, oil, machinery, aerospace, health care, daily cosmetics, food, agricultural avocation and even daily life, all obtained to use widely.In addition, dichloromethyl-tetramethyl disiloxane still do synthetic organosilicon liquid crystal main raw material (Zhang Xianliang, Zhang Jianqiang, Wang Chengrui, Zhuo Renxi, SCI, 1995,16,471-476).
The present invention generates on the basis of reference, (Tang, Hong-Ding in the former method for preparing dichloromethyl-tetramethyl disiloxane, Xiang Ying, Zhang, Xian-Liang, WuhanUniversity Journal Natural Sciences, 2000,5,233-237), chloromethyl-dimethylchlorosilane joined in 50% the ethanolic soln, continue backflow 6 hours again after being added dropwise to complete and make yield 83%.This method has been used ethanol, refluxes and has wasted the energy, and long reaction time, cost are very high.
Summary of the invention
The objective of the invention is to overcome the shortcoming of existing preparation dichloromethyl-tetramethyl disiloxane method, provide a kind of chloromethyl-dimethylchlorosilane hydrolysis to prepare the method for dichloromethyl-tetramethyl disiloxane.
The technical scheme that the present invention solves its technical problem employing is:
With chloromethyl-dimethylchlorosilane is raw material, directly dropping hydrolysis in water prepares dichloromethyl-tetramethyl disiloxane, need not heating, utilizes this reaction self heat release can finish reaction, temperature of reaction is controlled at 20～100 ℃, be added dropwise to complete postcooling to room temperature, isolate organic layer, organic layer is washed to neutrality, the organic layer drying, the fraction of 200～202 ℃ of boiling points, yield 95～98%, purity 97～99% are collected in distillation.
Reaction equation is as follows:
The method for preparing dichloromethyl-tetramethyl disiloxane of the present invention, the key of its technology are that chloromethyl-dimethylchlorosilane direct hydrolysis prepares dichloromethyl-tetramethyl disiloxane, utilize this reaction self heat release to finish reaction, do not need heating.
The present invention compares the beneficial effect that has with background technology: yield height of the present invention, raw material economize, energy-conservation, save time, cost is low, efficient is high, simple to operate, be fit to suitability for industrialized production.
Embodiment
Embodiment 1:
In the three-necked bottle that thermometer, reflux condensing tube, dropping funnel are housed, add 50mL water, drip 72 gram chloromethyl-dimethylchlorosilanes, control reaction temperature after being added dropwise to complete, is isolated organic layer at 20～30 ℃, organic layer is washed to neutrality, the organic layer anhydrous sodium sulfate drying filters, and the fraction of 200～202 ℃ of boiling points is collected in the product distillation, yield 95%, purity 97.6%.
Embodiment 2:
In the three-necked bottle that thermometer, reflux condensing tube, dropping funnel are housed, add 50mL water, drip 72 gram chloromethyl-dimethylchlorosilanes, control reaction temperature after being added dropwise to complete, is isolated organic layer at 30～40 ℃, organic layer is washed to neutrality, the organic layer anhydrous sodium sulfate drying filters, and the fraction of 200～202 ℃ of boiling points is collected in the product distillation, yield 96%, purity 97.3%.
Embodiment 3:
In the three-necked bottle that thermometer, reflux condensing tube, dropping funnel are housed, add 50mL water, drip 72 gram chloromethyl-dimethylchlorosilanes, control reaction temperature after being added dropwise to complete, is isolated organic layer at 40～50 ℃, organic layer is washed to neutrality, the organic layer anhydrous sodium sulfate drying filters, and the fraction of 200～202 ℃ of boiling points is collected in the product distillation, yield 96%, purity 98.1%.
Embodiment 4:
In the three-necked bottle that thermometer, reflux condensing tube, dropping funnel are housed, add 50mL water, drip 72 gram chloromethyl-dimethylchlorosilanes, control reaction temperature after being added dropwise to complete, is isolated organic layer at 50～60 ℃, organic layer is washed to neutrality, the organic layer anhydrous sodium sulfate drying filters, and the fraction of 200～202 ℃ of boiling points is collected in the product distillation, yield 96.5%, purity 98.5%.
Embodiment 5:
In the three-necked bottle that thermometer, reflux condensing tube, dropping funnel are housed, add 50mL water, drip 72 gram chloromethyl-dimethylchlorosilanes, control reaction temperature after being added dropwise to complete, is isolated organic layer at 60～70 ℃, organic layer is washed to neutrality, the organic layer anhydrous sodium sulfate drying filters, and the fraction of 200～202 ℃ of boiling points is collected in the product distillation, yield 98%, purity 97%.
Embodiment 6:
In the three-necked bottle that thermometer, reflux condensing tube, dropping funnel are housed, add 50mL water, drip 72 gram chloromethyl-dimethylchlorosilanes, control reaction temperature after being added dropwise to complete, is isolated organic layer at 70～80 ℃, organic layer is washed to neutrality, the organic layer anhydrous sodium sulfate drying filters, and the fraction of 200～202 ℃ of boiling points is collected in the product distillation, yield 95%, purity 97.9%.
Embodiment 7:
In the three-necked bottle that thermometer, reflux condensing tube, dropping funnel are housed, add 50mL water, drip 72 gram chloromethyl-dimethylchlorosilanes, control reaction temperature after being added dropwise to complete, is isolated organic layer at 80～100 ℃, organic layer is washed to neutrality, the organic layer anhydrous sodium sulfate drying filters, and the fraction of 200～202 ℃ of boiling points is collected in the product distillation, yield 95%, purity 98%.
Embodiment 8:
In the three-necked bottle that thermometer, reflux condensing tube, dropping funnel are housed, add 100mL water, drip 144 gram chloromethyl-dimethylchlorosilanes, control reaction temperature after being added dropwise to complete, is isolated organic layer at 50～60 ℃, organic layer is washed to neutrality, the organic layer anhydrous sodium sulfate drying filters, and the fraction of 200～202 ℃ of boiling points is collected in the product distillation, yield 96%, purity 99%.
Claims (1)
1. chloromethyl-dimethylchlorosilane hydrolysis prepares the method for dichloromethyl-tetramethyl disiloxane, it is characterized in that: with chloromethyl-dimethylchlorosilane is raw material, directly dropping hydrolysis in water prepares dichloromethyl-tetramethyl disiloxane, need not heating, utilize this reaction self heat release can finish reaction, temperature of reaction is controlled at 20～100 ℃, be added dropwise to complete postcooling to room temperature, isolate organic layer, organic layer is washed to neutrality, the organic layer drying, and the fraction of 200～202 ℃ of boiling points is collected in distillation, yield 95～98%, purity 97～99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710156556XA CN101157701A (en) | 2007-11-08 | 2007-11-08 | Method for preparing bischloromethyl-tetramethyl disiloxane by hydrolysis of chloromethyl-dimethylchlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200710156556XA CN101157701A (en) | 2007-11-08 | 2007-11-08 | Method for preparing bischloromethyl-tetramethyl disiloxane by hydrolysis of chloromethyl-dimethylchlorosilane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101157701A true CN101157701A (en) | 2008-04-09 |
Family
ID=39305949
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200710156556XA Pending CN101157701A (en) | 2007-11-08 | 2007-11-08 | Method for preparing bischloromethyl-tetramethyl disiloxane by hydrolysis of chloromethyl-dimethylchlorosilane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101157701A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351893A (en) * | 2011-10-19 | 2012-02-15 | 浙江大学 | Process for preparing tetramethyl-bis (N1-methylene-1, 2-ethylenediamine) disiloxane |
| CN103030809A (en) * | 2012-12-31 | 2013-04-10 | 山东大学 | Chloromethyl-containing polysiloxane and synthetic method thereof |
| CN110759938A (en) * | 2019-11-08 | 2020-02-07 | 山东大学 | Hydroxyalkyl disiloxane containing hetero atoms, preparation method and application thereof |
| CN110818735A (en) * | 2019-12-03 | 2020-02-21 | 江西蓝星星火有机硅有限公司 | Method for preparing 1,1,3, 3-tetramethyldisiloxane |
| CN111909191A (en) * | 2020-07-01 | 2020-11-10 | 鲁西化工集团股份有限公司硅化工分公司 | Method and system for preparing tetramethyl dihydrodisiloxane by hydrolyzing organosilicon low-boiling-point substances and comprehensive utilization method |
-
2007
- 2007-11-08 CN CNA200710156556XA patent/CN101157701A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102351893A (en) * | 2011-10-19 | 2012-02-15 | 浙江大学 | Process for preparing tetramethyl-bis (N1-methylene-1, 2-ethylenediamine) disiloxane |
| CN103030809A (en) * | 2012-12-31 | 2013-04-10 | 山东大学 | Chloromethyl-containing polysiloxane and synthetic method thereof |
| CN110759938A (en) * | 2019-11-08 | 2020-02-07 | 山东大学 | Hydroxyalkyl disiloxane containing hetero atoms, preparation method and application thereof |
| CN110818735A (en) * | 2019-12-03 | 2020-02-21 | 江西蓝星星火有机硅有限公司 | Method for preparing 1,1,3, 3-tetramethyldisiloxane |
| CN110818735B (en) * | 2019-12-03 | 2022-09-16 | 江西蓝星星火有机硅有限公司 | Method for preparing 1,1,3, 3-tetramethyldisiloxane |
| CN111909191A (en) * | 2020-07-01 | 2020-11-10 | 鲁西化工集团股份有限公司硅化工分公司 | Method and system for preparing tetramethyl dihydrodisiloxane by hydrolyzing organosilicon low-boiling-point substances and comprehensive utilization method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101157701A (en) | Method for preparing bischloromethyl-tetramethyl disiloxane by hydrolysis of chloromethyl-dimethylchlorosilane | |
| EP2543646A4 (en) | Luminous nano-glass-ceramics used as white led source and preparing method of luminous nano-glass-ceramics | |
| CN103086918A (en) | Toluylene nitrile derivative with D-A structure and synthesis method and application thereof | |
| CN102965735A (en) | Synthesis method of bismuth sulfide nanorod arrays with length-diameter ratios regulated and controlled by solvent hydrothermal method | |
| CN103467508A (en) | Preparation method of methyl ketone oxime methoxy silane | |
| Blevins et al. | Iron trichloride promoted hydrolysis of potassium organotrifluoroborates | |
| CN102351691A (en) | Method for synthesizing adipic acid monoethyl ester | |
| CN102267911A (en) | Synthesis method of methyl salicylate | |
| CN103626621B (en) | 1,2-dihydro cyclobutane is [α] naphthalene new synthetic method also | |
| CN101602714B (en) | Novel method for synthesizing 2-chloronicotinic acid | |
| CN101811985B (en) | Method for producing pentylcyclohexylbiphenylcarbonitrile | |
| CN101967102B (en) | Synthesizing method of N,N-diethyl-3,7-dimethyl-(E)-2,6-octadiene-1-amine | |
| CN104030995B (en) | The main body macro ring built by triphenylamine and many side shoots triphenylamine hole mobile material | |
| CN104356073B (en) | A kind of microwave-assisted efficiently synthesizes the method for 5-cyanogen uracil | |
| CN2817945Y (en) | Stepped sublimator | |
| CN102219739A (en) | Azaanthracene compound and synthesizing method thereof | |
| CN103172506B (en) | A kind of take nano cupric oxide as the method for catalyst preparing croconic acid | |
| CN206715358U (en) | A kind of OLED material sublimation purifying plants | |
| CN103073407A (en) | Method for preparing 2, 4-dihydroxy benaophenonel by using indium trichloride to catalyze | |
| CN101830833B (en) | Method for refining medicinal urea | |
| CN100551926C (en) | 1,1,3,3-tetramethyl--5-(2-amido ethyl)-1,3-two silicon-2-Evil-5-piperidine preparation method | |
| CN204485865U (en) | A kind of Far-infrared Heating reactor | |
| CN208944128U (en) | A kind of biotechnology equipment for purifying | |
| CN102633756A (en) | Novel method for synthetizing alpha-furylacrylic acid | |
| CN102351834B (en) | Economic, practical, and environment friendly method for preparing norathyriol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080409 |