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Method for synthesizing di-alkyl chlorosilane

A technology of monochlorosilane and synthesis method, which is applied in the synthesis of dialkyl monochlorosilane and the synthesis field of organosilicon compounds, can solve the problems of low synthesis yield, complicated process route and post-processing, and achieves high product yield , high yield, easy to achieve effect

Inactive Publication Date: 2015-09-09
CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of this invention is to provide a kind of new method of synthesizing dialkyl chlorosilane, this method can overcome to a certain extent the synthesis yield of dialkyl chlorosilane in the prior art is lower, operational route and aftertreatment complex the puzzle

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 41.50g of the mixture of aluminum hydride and aluminum chloride (the molar ratio of aluminum hydride and aluminum chloride is 8:1) into a container containing 420g of N,N-dimethylimidazolidinone and equipped with a reflux device for condensation, Stir for 10 minutes, add 125g of raw materials (CH 3 ) 2 SiCl 2 , The stirring reaction was carried out at a temperature of 90°C for 2.5 hours. Then the reaction temperature was increased to 130°C, and stirring was continued for 40 minutes to stop the reaction. After the reaction mixture is filtered and distilled, dimethyl monochlorosilane can be obtained.

[0025] Tests show that the yield of dimethyl monochlorosilane obtained in this example is 65%.

Embodiment 2

[0027] Add 41.50g of the mixture of aluminum hydride and aluminum chloride (the molar ratio of aluminum hydride and aluminum chloride is 8:1) into a container containing 480g of N,N-dimethylimidazolidinone and equipped with a reflux device for condensation, Stir for 10 minutes, add 153g of raw materials (CH 2 CH 3 ) 2 SiCl 2 , The stirring reaction was carried out at a temperature of 90°C for 2.5 hours. Then the reaction temperature was increased to 130°C, and stirring was continued for 40 minutes to stop the reaction. After the reaction mixture is filtered and distilled, diethylmonochlorosilane can be obtained.

[0028] Tests show that the yield of diethylmonochlorosilane obtained in this example is 63%.

Embodiment 3

[0030] Add 41.50g of the mixture of aluminum hydride and aluminum chloride (the molar ratio of aluminum hydride to aluminum chloride is 8:1) into a container containing 520g of N,N-dimethylimidazolidinone and equipped with a reflux device for condensation, Stir for 10 minutes, add 181g of raw materials (CH 2 CH 2 CH 3 ) 2 SiCl 2 , The stirring reaction was carried out at a temperature of 90°C for 2.5 hours. Then the reaction temperature was increased to 130°C, and stirring was continued for 40 minutes to stop the reaction. After the reaction mixture is filtered and distilled, dipropyl monochlorosilane can be obtained.

[0031] Tests show that the yield of dipropyl monochlorosilane obtained in this example is 63%.

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Abstract

The invention discloses a method for synthesizing di-alkyl chlorosilane. The method includes the following steps: adding a reducing agent A into a container containing a solvent B and a reflux condenser, wherein the mass ratio of the reducing agent A to the solvent B is (1:10)-(1:90), stirring for 10-20 minutes, adding an equimolar amount of a raw material C within 16-20 minutes of stirring for reaction at 55-90 DEG C, stirring and reacting for 2-3 hours, wherein the structural formula of the raw material C is (Rf) 2SiCl2, and Rf is methyl, ethyl, propyl or butyl; increasing the reaction temperature to 120-130 DEG C, stirring for 40-60 minutes and stopping the reaction; filtering and distilling the mixture after reaction. The solvent B is one or more of methyl pyrrolidone, ethyl pyrrolidone, and N,N-dimethyl imidazolidinone, the reducing agent A is one or more of aluminum hydride / aluminum chloride, lithium aluminum hydride / chloride aluminum, sodium hydride / aluminum chloride and aluminum hydride / lithium aluminum hydride. The reaction process and post-treatment are simple, the synthetic yield is high, and the raw material cost is low.

Description

Technical field [0001] The invention relates to a method for synthesizing organosilicon compounds, in particular to a method for synthesizing dialkyl monochlorosilane, which belongs to the technical field of organic synthesis. Background technique [0002] Dialkyl monochlorosilane is one of the very important monomers in the synthesis of silicone polymers. Its production level and device scale are important basis for measuring a country's organic silicon technology level. [0003] At present, the main methods for synthesizing dialkyl monochlorosilanes are: direct method, Griya method, high boiling point cracking method, redistribution method and alkylchlorosilane reduction method. The direct synthesis method, due to its low yield, hinders its commercialization process. The post-processing of Griya method and redistribution method is more complicated. The high boiling point cracking method requires stricter equipment. Due to its high yield, the methylchlorosilane reduction metho...

Claims

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Application Information

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IPC IPC(8): C07F7/12
Inventor 司林旭司志红
Owner CHANGSHU 3F ZHONGHAO NEW CHEM MATERIALS
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