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Method for preparing methyltris(trimethylsiloxy)silane

A technology of trimethylsiloxane and methyltrialkoxysilane, which is applied in the field of preparation of methyltrisilane, and can solve the problems of high acid water discharge and low yield

Inactive Publication Date: 2019-08-09
济南雅达新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, it is commonly used at present to prepare by co-hydrolysis of trimethylchlorosilane and methyltrichlorosilane; methyltrimethoxy or triethoxysilane, and hexamethyldisiloxane in strong acid macropore Prepared by exchange resin; hexamethyldisiloxane and methyltrimethoxy or triethoxysilane are co-hydrolyzed in an acidic organic solvent, but the yield is relatively low, and there is acid water discharge in the chlorosilane method more volume problem

Method used

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  • Method for preparing methyltris(trimethylsiloxy)silane

Examples

Experimental program
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Embodiment 1

[0040] 486 grams of hexamethyldisiloxane and 64 grams of isopropanol were cooled to below 10°C while mixing, and 0.4 grams of 5% dichloromethane solution of oxygen-containing linear phosphazene chloride was added dropwise in 15 minutes, and the drops were completed Subsequent stirring for 30 minutes, then 136.2 grams of methyltrimethoxysilane was added dropwise over 30 minutes and continued to stir for 1 hour, and then at 5-10 ° C, 105 grams of water was added dropwise over 1 hour, and after the drop was completed, the temperature was 20-25 °C for 3 hours. Then add 0.68 g of ammonium bicarbonate, neutralize at 80-100° C. for 2 hours, cool down and filter, static layering, take several layers of distillation, and collect 120-125° C. (the fraction at 12kpa). Obtain 293 grams of methyl tri(trimethylsiloxane) silane product which is transparent, colorless, tasteless and nontoxic. Product performance: purity 99.6%, yield 94.5%, boiling point: 190°C, freezing point -74°C, viscosity...

Embodiment 2

[0042] 324 grams of hexamethyldisiloxane and 96 grams of isopropanol were cooled to below 10°C while mixing, and 0.6 grams of a 5% dichloromethane solution of oxygen-containing linear phosphazene chloride was added dropwise in 30 minutes, and the drops were completed Subsequent stirring for 60 minutes, and then 136.2 grams of methyltrimethoxysilane was added dropwise over 30 minutes, and continued to stir for 2 hours, and then at 5-25 ° C, 105 grams of water was added dropwise over 1 hour, and after the drop was completed, it was added at 15- The reaction was continued at -20°C for 4.5 hours. Then add 1 gram of ammonium bicarbonate, neutralize at 80-100° C. for 2 hours, cool down and filter, stand still and separate layers, take several layers of distillation, and collect 120-125° C. (the fraction at 12kpa). Obtain 289 grams of methyl tri(trimethylsiloxane) silane product which is transparent, colorless, tasteless and nontoxic. The product properties are: purity 99.5%, yield ...

Embodiment 3

[0044] 648 grams of hexamethyldisiloxane and 120 grams of isopropanol were cooled to below 10°C while mixing, and 0.82 grams of 5% dichloromethane solution of oxygen-containing linear phosphazene chloride was added dropwise in 40 minutes, and the drops were completed Subsequent stirring for 60 minutes, and then 272 grams of methyltrimethoxysilane was added dropwise over 60 minutes, and continued to stir for 4 hours, then at 5-25 ° C, 210 grams of water was added dropwise over 2 hours. The reaction was continued at -20°C for 5 hours. Then add 1.5 g of ammonium bicarbonate, neutralize at 80-100° C. for 3 hours, cool down and filter, static layering, take several layers of distillation, and collect 120-125° C. (the fraction at 12kpa). Obtain 601 grams of methyl tri(trimethylsiloxane) silane product which is transparent, colorless, tasteless and nontoxic. The purity is 99.7%, and the yield is 96.9%.

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Abstract

The invention provides a method for preparing methyltris(trimethylsiloxy)silane. The method comprises the steps that hexamethyldisiloxane and alcohol are mixed, then oxygen-containing linear phosphazene chloride is dripped in the mixture, and stirring is conducted; methyl trialkoxysilane is dripped in the mixture, and stirring is conducted; water is dripped in the mixture, and reacting is conducted; neutralization and filtration are conducted, and standing and layering are conducted to obtain an organic layer and a water layer; the organic layer is distilled, and the methyltris(trimethylsiloxy)silane is obtained. The prepared methyltris(trimethylsiloxy)silane is high in yield, and waste liquid discharge is very less.

Description

technical field [0001] This application relates to but not limited to the field of material chemistry, especially to but not limited to the preparation method of methyl tri(trimethylsiloxane) silane. Background technique [0002] Traditional dry cleaning agents are toxic perchlorethylene, which is widely used because of its low cost and low price. The application of new-generation petroleum detergents and liquid carbon dioxide detergents is greatly restricted due to high cost and equipment update problems. In the cleaning of circuit boards and equipment in the electronics industry, CF-113 is highly polluting to the environment and harmful to the human body. Methyl tri(trimethylsiloxane) silane (hereinafter referred to as M 3 T), moderate cost, non-toxic and tasteless, safe to use, is an environmentally friendly and safe substitute at present. [0003] In the cosmetics, skin care, and hair care industries, decamethylcyclopentasiloxane (D 5 ) is one of the essential carrie...

Claims

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Application Information

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IPC IPC(8): C07F7/08
CPCC07F7/0838C07F7/0874
Inventor 赵秀华
Owner 济南雅达新材料科技有限公司