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Preparation method of phenyl alkoxy silane

A technology of phenylalkoxysilane and alkoxysilane, which is applied in the field of preparation of phenylalkoxysilane, can solve the problems of danger and strict raw material requirements, achieve mild reaction conditions and reduce the number of rectification steps Effect

Pending Publication Date: 2022-03-08
HUBEI XINGRUI SILICON MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem of strict and dangerous raw materials in the preparation of phenylalkoxysilane, the reaction of alkoxydisilane, halogenated benzene and strong organic base is used to prepare phenylalkoxysilane

Method used

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  • Preparation method of phenyl alkoxy silane
  • Preparation method of phenyl alkoxy silane
  • Preparation method of phenyl alkoxy silane

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Add 400g of methyltrimethoxysilane and 1.1mol of sodium methoxide into the reaction kettle, pass through nitrogen protection, stir evenly, and maintain the temperature at 20°C, and then add 1.2mol of chlorobenzene and dimethyltetramethoxydimethoxide dropwise at the same time Silane 1mol. Add dropwise for 2h and continue the reaction for 6h. The reaction liquid after the reaction is first filtered, and the filtrate is separated by rectification to separate methylphenyldimethoxysilane and methyltrimethoxysilane. The yield of methylphenyldimethoxysilane is 45.6%, and the yield of methyltrimethoxysilane is 95.7%.

Embodiment 2

[0021] Add 250 g of tetraethyl silicate and 1.2 mol of sodium ethoxide into the reaction kettle, pass through helium protection, stir evenly, and maintain the temperature at 35 ° C, and then add 1 mol of chlorobenzene and 1 mol of hexaethoxydisilane dropwise at the same time. Add dropwise for 3h and continue the reaction for 5h. The reaction liquid after the reaction is first filtered, and the filtrate is separated by rectification to separate phenyltriethoxysilane and tetraethyl silicate. The yield of phenyltriethoxysilane is 40.6%, and the yield of tetraethyl silicate is 93.4%.

Embodiment 3

[0023] Add 300 g of dimethyldimethoxysilane and 1 mol of potassium methylate into the reaction kettle, pass through nitrogen protection, stir evenly, and maintain the temperature at 50 ° C, and then add 1.1 mol of bromobenzene and tetramethyldimethoxy Disilane 1mol. Add dropwise for 4h and continue the reaction for 4h. The reaction liquid after the reaction is first filtered, and the filtrate is separated by rectification to separate dimethylphenylmethoxysilane and dimethyldimethoxysilane. The yield of dimethylphenylmethoxysilane is 60.7%, and the yield of dimethyldimethoxysilane is 98.8%.

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Abstract

The invention discloses a preparation method of phenyl alkoxy silane, which comprises the following steps: adding alkoxy silane and organic strong base into a reaction kettle, introducing inert gas for protection, uniformly stirring, maintaining the temperature at 20-60 DEG C, and simultaneously and respectively dropwise adding halogenated benzene and alkoxy substituted disilane. Dropwise adding for 2-4 hours, and continuously reacting for 4-6 hours; and filtering the reaction liquid after the reaction, and rectifying the filtrate to separate phenyl alkoxy silane and alkoxy silane. According to the invention, alkoxy silane is used as a solvent, can effectively dissolve organic strong base, has good intersolubility with halogenated benzene and alkoxy disilane, and is beneficial to the proceeding of the reaction. Reaction conditions are mild, safe and easy to operate.

Description

technical field [0001] The invention relates to a preparation method of organosilane, more particularly to a preparation method of phenylalkoxysilane. Background technique [0002] Phenylalkoxysilane refers to a special monomer with two functional groups, phenyl and alkoxy, directly linked to the silicon atom. Phenyl alkoxysilane is an important organosilicon compound, and it is one of the main raw materials for preparing phenyl silicone resin, phenyl silicone oil, and phenyl silicone rubber. It can improve the performance of organosilicon polymers, especially heat resistance The role of resistance, radiation resistance, chemical stability, refractive index, etc. is very obvious. With the development of the silicone industry and the expansion of the application field of silicone, the demand for phenylsilane is growing rapidly. [0003] The preparation of phenylalkoxysilane mainly includes Grignard reagent method, sodium condensation method, and alcoholysis method. Among t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08G77/04C08G77/06
CPCC07F7/1804C07F7/1876C07F7/188C08G77/04C08G77/06
Inventor 李书兵杜斌王文金沈谦辛梓杰匡建国姚中鹏
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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