CN101362778B - Preparation method of chloromethyl-oxyethyl-dimethylsilane - Google Patents
Preparation method of chloromethyl-oxyethyl-dimethylsilane Download PDFInfo
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- CN101362778B CN101362778B CN2008101616015A CN200810161601A CN101362778B CN 101362778 B CN101362778 B CN 101362778B CN 2008101616015 A CN2008101616015 A CN 2008101616015A CN 200810161601 A CN200810161601 A CN 200810161601A CN 101362778 B CN101362778 B CN 101362778B
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- chloromethyl
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- siloxane
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Abstract
The invention discloses a method for preparing chloromethyl-oxethyl-dimethyl siloxane. The method takes chloromethyl-dimethyl-siloxane and absolute ethyl alcohol as raw materials which are stirred; the absolute ethyl alcohol is added to the chloromethyl-dimethyl-siloxane in a dropwise manner; the mole ratio of the chloromethyl-dimethyl-siloxane to the absolute ethyl alcohol is 1:1.2-1.5; the reaction temperature is controlled to be 20 DEG C to 60 DEG C; after adding in a dropwise way, reaction is carried out fully; during the reaction process, nitrogen is blown in for blowing away chlorine hydride gas; after reaction, a product is distilled, and distillate fractions at the temperature of 132 DEG C to 133 DEG C are collected. During the reaction process, the chlorine hydride gas which is blown away is adsorbed by water and diluted alkali in sequence, thus being capable of realizing discharge without pollution. The method has the advantages of saving raw materials, saving time, low cost, simple operation, being suitable for industrialized production, and the like, and product yield reaches as high as 90 percent to 93 percent and purity reaches more than 95 percent.
Description
Technical field
The present invention relates to prepare the method for chloromethyl-oxyethyl-dimethylsilane.
Background technology
Organosilicon product has high-low temperature resistant, electric insulation, anti-ozone, radiation hardness, difficult combustion, hydrophobic, corrosion-resistant, nonpoisonous and tasteless and physiology inertia etc., be widely used in every profession and trades such as electric, building, weaving, light industry, medical treatment, and also have a wide range of applications in automobile industry.
Not domestic not the appearing in the newspapers of preparation of at present relevant chloromethyl-oxyethyl-dimethylsilane.(Steven P.Hopper in the former method for preparing similar compound chloromethyl-methoxyl group-dimethylsilane, Michael J.Tremelling, EmmaW.Goldman, Journal of Organometallic Chemistry, 1980,190 (3), 247-56), use lithium methoxide, sodium methylate, potassium methylate respectively and chloromethyl-dimethyl-chlorosilane reaction, the yield of reaction is respectively 94%, 54%, 17%.But the reaction unit complexity that is to use, and these metal methoxide things are relatively expensive, and chloromethyl-dimethyl-chlorosilane need present gaseous state and could react, so cost is very high, is not suitable for large batch of suitability for industrialized production.
Summary of the invention
The purpose of this invention is to provide a kind of raw material and economize, energy-conservation, cost is low, efficient height, the method for preparing chloromethyl-oxyethyl-dimethylsilane of suitable suitability for industrialized production.
The method for preparing chloromethyl-oxyethyl-dimethylsilane of the present invention, its step is as follows:
Stir down dehydrated alcohol is added drop-wise in chloromethyl-dimethyl-chlorosilane, the mol ratio of chloromethyl-dimethyl-chlorosilane and dehydrated alcohol is 1:1.2～1.5, control reaction temperature is at 20～60 ℃, after dropwising, fully reaction, advertise nitrogen in the reaction process and blow and catch up with hydrogen chloride gas, 132-133 ℃ fraction is collected in the distillation of reaction after product.
Reaction equation is as follows:
Be the hydrogen chloride gas discharging after water, diluted alkaline absorb successively that realizes non-pollution discharge, will blow in the reaction process of the present invention catching up with.
Beneficial effect of the present invention is:
The present invention prepares chloromethyl-oxyethyl-dimethylsilane with the direct ethanolysis of chloromethyl-dimethyl-chlorosilane, has overcome to use expensive reagent and complicated reaction unit.Have province's raw material, energy-conservation, save time, cost is low, simple to operate, be fit to advantages such as suitability for industrialized production, and product yield is up to 90～93%, purity is more than 95%.
Embodiment
Embodiment 1:
Reflux condensing tube is being housed, add raw material chloromethyl-dimethyl-chlorosilane 143g (1mol) in the reaction flask of dropping funnel, Dropwise 5 9.8g (1.2mol) dehydrated alcohol, control reaction temperature is at 20～30 ℃, and advertise nitrogen and catch up with the hydrogen chloride gas of generation (first water absorbs and produces hydrochloric acid, absorb with diluted alkaline again, realize non-pollution discharge).After dropwising, continue reaction 1h, 132-133 ℃ fraction is collected in the distillation of reaction after product.Yield 90.2%, purity 95.0%.
Embodiment 2:
Reflux condensing tube is being housed, add raw material chloromethyl-dimethyl-chlorosilane 143g (1mol) in the reaction flask of dropping funnel, Dropwise 5 9.8g (1.3mol) dehydrated alcohol, control reaction temperature is at 30～40 ℃, and advertise nitrogen and catch up with the hydrogen chloride gas of generation (first water absorbs and produces hydrochloric acid, absorb with diluted alkaline again, realize non-pollution discharge).After dropwising, continue reaction 1h, 132-133 ℃ fraction is collected in the distillation of reaction after product.Yield 93.0%, purity 95.3%.
Embodiment 3:
Reflux condensing tube is being housed, add raw material chloromethyl-dimethyl-chlorosilane 143g (1mol) in the reaction flask of dropping funnel, Dropwise 5 9.8g (1.3mol) dehydrated alcohol, control reaction temperature is at 40～50 ℃, and advertise nitrogen and catch up with the hydrogen chloride gas of generation (first water absorbs and produces hydrochloric acid, absorb with diluted alkaline again, realize non-pollution discharge).After dropwising, continue reaction 1h, 132-133 ℃ fraction is collected in the distillation of reaction after product.Yield 92.1%, purity 95.6%.
Embodiment 4:
Reflux condensing tube is being housed, add raw material chloromethyl-dimethyl-chlorosilane 143g (1mol) in the reaction flask of dropping funnel, Dropwise 5 9.8g (1.3mol) dehydrated alcohol, control reaction temperature is at 50～60 ℃, and advertise nitrogen and catch up with the hydrogen chloride gas of generation (first water absorbs and produces hydrochloric acid, absorb with diluted alkaline again, realize non-pollution discharge).After dropwising, continue reaction 1h, 132-133 ℃ fraction is collected in the distillation of reaction after product.Yield 92.6%, purity 95.2%.
Embodiment 5:
Reflux condensing tube is being housed, add raw material chloromethyl-dimethyl-chlorosilane 143g (1mol) in the reaction flask of dropping funnel, drip 69g (1.5mol) dehydrated alcohol, control reaction temperature is at 30～40 ℃, and advertise nitrogen and catch up with the hydrogen chloride gas of generation (first water absorbs and produces hydrochloric acid, absorb with diluted alkaline again, realize non-pollution discharge).After dropwising, continue reaction 1h, 132-133 ℃ fraction is collected in the distillation of reaction after product.Yield 92.4%, purity 95.7%.
Claims (2)
1. method for preparing chloromethyl-oxyethyl-dimethylsilane is characterized in that step is as follows:
Stir down dehydrated alcohol is added drop-wise in chloromethyl-dimethyl-chlorosilane, the mol ratio of chloromethyl-dimethyl-chlorosilane and dehydrated alcohol is 1:1.2～1.5, control reaction temperature is at 20～60 ℃, after dropwising, fully reaction, advertise nitrogen in the reaction process and blow and catch up with hydrogen chloride gas, 132-133 ℃ fraction is collected in the distillation of reaction after product.
2. the method for preparing chloromethyl-oxyethyl-dimethylsilane according to claim 1 is characterized in that the hydrogen chloride gas discharging after water, diluted alkaline absorb successively of catching up with blowing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101616015A CN101362778B (en) | 2008-09-16 | 2008-09-16 | Preparation method of chloromethyl-oxyethyl-dimethylsilane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101616015A CN101362778B (en) | 2008-09-16 | 2008-09-16 | Preparation method of chloromethyl-oxyethyl-dimethylsilane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101362778A CN101362778A (en) | 2009-02-11 |
| CN101362778B true CN101362778B (en) | 2011-06-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2008101616015A Expired - Fee Related CN101362778B (en) | 2008-09-16 | 2008-09-16 | Preparation method of chloromethyl-oxyethyl-dimethylsilane |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115558366B (en) * | 2022-10-28 | 2024-03-26 | 浙江中通汽车零部件有限公司 | Synthetic resin coating for high-stability connecting nut and coating process thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2511056A (en) * | 1947-07-01 | 1950-06-13 | Dow Corning | Organo siloxanes and their production |
| US4228092A (en) * | 1978-01-02 | 1980-10-14 | Dynamit Nobel Aktiengesellschaft | Process for the preparation of organoalkoxysilanes |
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2008
- 2008-09-16 CN CN2008101616015A patent/CN101362778B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2511056A (en) * | 1947-07-01 | 1950-06-13 | Dow Corning | Organo siloxanes and their production |
| US4228092A (en) * | 1978-01-02 | 1980-10-14 | Dynamit Nobel Aktiengesellschaft | Process for the preparation of organoalkoxysilanes |
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| CN101362778A (en) | 2009-02-11 |
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Effective date of registration: 20110425 Address after: 310027 Hangzhou, Zhejiang Province, Xihu District, Zhejiang Road, No. 38, No. Applicant after: Zhejiang University Co-applicant after: Ningbo Economic and Technical Development Zone SICO New Material Co.,Ltd. Address before: 310027 Hangzhou, Zhejiang Province, Xihu District, Zhejiang Road, No. 38, No. Applicant before: Zhejiang University |
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