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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 convenient operation

Inactive Publication Date: 2015-01-07
HUBEI XINGFA CHEM GRP CO LTD
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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

[0019] Add 200.1g of anhydrous water to a 1000ml four-necked 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 of 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 room temperature, ammonia gas is introduced to neutr...

Embodiment 2

[0021] Add 205.3g of anhydrous water to a 1000ml four-necked 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 of 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 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 room temperature, ammonia gas is introduced to neutralize to ...

Embodiment 3

[0023] Add 203.5g of anhydrous water to a 1000ml 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 of 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 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 room temperature, ammonia gas is introduced to neutrali...

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PUM

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Abstract

The invention provides a preparation method of methyltrialkoxysilane. The preparation method comprises the following steps of adding anhydrous alcohol into a reaction container A, arranging one end of a gas-guide tube under the liquid level in the reaction container A, introducing the other end of the gas-guide tube into a container B with methyltrichlorosilane, heating the anhydrous alcohol in the reaction container A to a temperature of 55-63 DEG C for a reaction, heating the methyltrichlorosilane in the container B to a temperature of 62-68 DEG C, feeding N2 into the container B, heating the mixed solution in the reaction container A to a temperature of 75-88 DEG C, carrying out a backflow thermal-insulation reaction process for 1-4h, then stopping heating, collecting the product, and feeding ammonia gas into the product to adjust product pH to 8-9 so that methyltrialkoxysilane is obtained. Dry neutral gas and an ammonia gas neutralizer are used under the conditions of normal pressure and low temperature. The preparation method utilizes simple technical equipment, is convenient for operation, and has a low cost and a high yield. Ammonium chloride obtained by neutralization of the preparation method can be 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): C07F7/18C01C1/16
Inventor 汪民康李永刚陈海平苗刚马会娟
Owner HUBEI XINGFA CHEM GRP CO LTD
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