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Preparation method of methyltrialkoxysilane

A technology of methyltrialkoxysilane and methyltrichlorosilane is applied in the field of preparation of improving the yield of methyltrialkoxysilane, and can solve the problems of high product cost, high raw material cost or high process equipment requirements , to achieve the effect of low price, high yield and reducing by-products

Inactive Publication Date: 2018-04-03
青岛九洲千和机械有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are also corresponding reports in China, such as Li Wenjia, Ji Chengjie, etc. reported in CN 1320600A in 2000, in the presence of petroleum ether in the laboratory, vinyltrimethoxysilane was prepared by two-way dropwise addition of vinyltrichlorosilane and methanol; In 2003, He Jun and Liu Yunmei used petroleum ether as a solvent to prepare trimethoxysilane, etc. in the laboratory. Most of their reaction methods were dropwise reaction, and the cost of raw materials used or the requirements for process equipment were high, resulting in high product costs. No, it is urgent to find a method with low raw material cost, simple process and high yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 200.1 g of anhydrous water to a 1000 ml four-neck flask A equipped with a thermometer, a mechanical stirrer, an air guide tube and a spherical condenser (the upper end of which is equipped with a serpentine condenser tube for feeding ice-salt water, a buffer bottle and an HCl absorption device). Ethanol, according to the molar ratio of methyl trichlorosilane: mass fraction is 99.5% absolute ethanol = 1:2.9, one end of the gas guide tube is connected below the liquid level of the reaction solution in A, and the other end of the gas guide tube is connected to dry nitrogen Add methyltrichlorosilane to a 250ml three-neck flask B, heat A to 60°C, turn on the ice-salt water cooling water, and heat B to 65°C at the same time, when the methyltrichlorosilane boils, pass dry nitrogen into B, After the feeding is completed, the temperature of A is raised to 80°C, and the heating is stopped after reflux for 3 hours. After cooling to normal temperature, ammonia gas is passed thro...

Embodiment 2

[0018] Add 205.3 g of anhydrous water to a 1000 ml four-neck flask A equipped with a thermometer, a mechanical stirrer, an air guide tube and a spherical condenser (the upper end of which is equipped with a serpentine condenser tube for feeding ice-salt water, a buffer bottle and an HCl absorption device). Ethanol, according to the molar ratio of methyl trichlorosilane: mass fraction is 99.5% absolute ethanol = 1:3.0, one end of the gas guide tube is connected below the liquid level of the reaction solution in A, and the other end of the gas guide tube is connected to dry nitrogen Add methyltrichlorosilane to a 500ml three-neck flask B, heat A to 60°C, turn on ice brine cooling water, and heat B to 65°C at the same time, when the methyltrichlorosilane boils, pass dry nitrogen into B, After the addition is completed, the temperature of A is raised to 80°C, and the heating is stopped after reflux for 3 hours. After cooling to normal temperature, ammonia gas is passed through to n...

Embodiment 3

[0020] Add 203.5 g of anhydrous water to a 1000 ml four-neck flask A equipped with a thermometer, a mechanical stirrer, an air duct and a spherical condenser (the upper end of which is equipped with a serpentine condenser tube for feeding ice-salt water, a buffer bottle and an HCl absorption device). Ethanol, according to the molar ratio of methyl trichlorosilane: mass fraction is 99.5% anhydrous methanol = 1:3.1, one end of the gas guide tube is connected below the liquid level of the reaction solution in A, and the other end of the gas guide tube is connected to dry nitrogen Add methyltrichlorosilane to a 500ml three-neck flask B, heat A to 60°C, turn on ice brine cooling water, and heat B to 65°C at the same time, when the methyltrichlorosilane boils, pass dry nitrogen into B, After the addition is completed, the temperature of A is raised to 80 ° C, and the heating is stopped after reflux for 3 hours. After cooling to room temperature, ammonia gas is introduced to neutraliz...

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Abstract

The invention provides a method for preparing methyltrialkoxysilane. Anhydrous alcohol is added into reaction vessel A, one end of the airway is connected below the liquid level of reaction vessel A, and the other end of the airway is connected to a In the container B of chlorosilane; heat the absolute alcohol in the reaction container A to 55-63 °C, heat the methyltrichlorosilane in the container B to 62-68 °C, and pass N2 into the container B to react The mixed solution in container A is heated to 75-88°C, refluxed and incubated for 1-4h; after refluxed and incubated for 1-4h, the heating is stopped to obtain the product, which is neutralized with ammonia gas until the pH is 8-9 to obtain methyl trialkoxysilane. In the present invention, under normal pressure and low temperature conditions, feeding dry neutral gas and adopting ammonia gas as a neutralizing agent, the process equipment is simple, easy to operate, low in price, high in yield, and the ammonium chloride produced after neutralization can be It is used as fertilizer and is conducive to green production.

Description

technical field [0001] The invention relates to a preparation method of alkoxysilane, in particular to a preparation method for improving the yield of methyltrialkoxysilane. Background technique [0002] Methyl trialkoxy silane is an important intermediate for the preparation of polysiloxane, mainly used in silicone rubber crosslinking agent, modified synthetic resin, fire retardant, plastic hard coating primer, water repellent, has great application value and broad market. The current preparation method of methyltrialkoxysilane is obtained by esterifying methyltrichlorosilane and anhydrous alcohol, neutralizing, filtering and distilling. There are also corresponding reports in China, such as Li Wenjia, Ji Chengjie, etc. reported in CN 1320600A in 2000, in the presence of petroleum ether in the laboratory, vinyltrimethoxysilane was prepared by two-way dropwise addition of vinyltrichlorosilane and methanol; In 2003, He Jun and Liu Yunmei used petroleum ether as a solvent to...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/188
Inventor 李辉
Owner 青岛九洲千和机械有限公司
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