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Preparation method of ethyl trimethoxy silane

The technology of ethyltrimethoxysilane and trimethoxysilane is applied in the field of preparation of intermediate ethyltrimethoxysilane, which can solve the difficulty of separation and purification of ethyltrimethoxysilane, increase the investment cost of rectifying tower equipment, Increase the operating costs of the separation process, and achieve the effects of low price, saving operating costs, and easy separation

Inactive Publication Date: 2010-06-16
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The atmospheric boiling point of tetramethoxysilane is 121°C. Compared with the atmospheric boiling point of ethyltrimethoxysilane of 124°C, the difference between the two is only 3°C, which makes the separation and purification of ethyltrimethoxysilane very difficult. In order to obtain high-purity ethyltrimethoxysilane, the number of plates in the rectification tower and the reflux ratio of the operation must be increased, which not only increases the load of rectification, increases the investment cost of rectification tower equipment, but also increases the separation process. operating costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1, the steps are:

[0029] 1) Add 1471.5 g of raw material trimethoxysilane, catalyst RuCl 3 ·xH 2 O 0.0220g, cocatalyst I 2 0.0804g;

[0030] 2) After stirring at room temperature for half an hour, feed 0.3MPa ethylene gas into the synthesis kettle from the gas insertion tube, and after the reaction is initiated, keep the reaction temperature at 80-100°C and stir the reaction;

[0031] 3) When the ethylene inlet valve is closed and the pressure in the synthesis kettle no longer decreases, the reaction is stopped, the material in the kettle is lowered to room temperature and collected, and the sample is analyzed by gas chromatography GC (HP-5 chromatographic column, column temperature 120°C, vaporization chamber 220°C, sampling chamber 220°C, FID detector), the content of ethyltrimethoxysilane is 94.94%, and the content of tetramethoxysilane is 1.58%. Calculate the ratio of ethyltrimethoxysilane and tetramethoxysilane The mass concentration ratio coeffic...

Embodiment 2

[0035] Embodiment 2, the steps are:

[0036] 1) Add 1401.5 g of raw material trimethoxysilane, catalyst RuCl 3 ·xH 2 O 0.0195g, cocatalyst I 2 0.1471g;

[0037] 2) After stirring at room temperature for half an hour, feed 0.3MPa ethylene gas into the synthesis kettle from the gas insertion tube, and after the reaction is initiated, keep the reaction temperature at 40-60°C and stir the reaction;

[0038] 3) When the ethylene inlet valve is closed and the pressure in the synthesis kettle no longer decreases, the reaction is stopped, the material in the kettle is lowered to room temperature and collected, and the sample is analyzed by gas chromatography GC (HP-5 chromatographic column, column temperature 120°C, vaporization chamber 220°C, sample chamber 220°C, FID detector), the content of ethyltrimethoxysilane is 93.80%, and the content of tetramethoxysilane is 2.18%. Calculate the ratio of ethyltrimethoxysilane to tetramethoxysilane The mass concentration ratio coefficient...

Embodiment 3

[0043] Add raw material trimethoxysilane 1445.9g, catalyst RuCl 3 ·xH 2 O 0.0381g, cocatalyst I 2 0.1520g, after stirring at room temperature for half an hour, pass 0.3MPa ethylene gas into the synthesis kettle from the gas bottom pipe, after the reaction is initiated, keep the reaction temperature at 50-70°C and stir the reaction; after closing the ethylene inlet valve, the synthesis kettle When the internal pressure no longer decreases, the reaction is stopped, the materials in the kettle are lowered to room temperature and collected, and the samples are analyzed by gas chromatography GC (HP-5 chromatographic column, column temperature 120°C, vaporization chamber 220°C, sampling chamber 220°C, FID detection device), the content of ethyltrimethoxysilane is 94.14%, and the content of tetramethoxysilane is 1.82%. The mass concentration ratio coefficient β of ethyltrimethoxysilane and tetramethoxysilane is calculated to be 51.73. The target product ethyltrimethoxysilane was o...

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Abstract

The invention relates to a preparation method of ethyl trimethoxy silane, aiming at solving the technical problem that a process and a device can be simple, usage and cost of a catalyst can be reduced, synthetic yield can be improved and desired products can be easy to be separated without adding additional solvent. The method in the invention comprises the following steps: 1) adding trimethoxy silane, catalyst and cocatalyst to a pressure-proof reaction kettle, wherein the mass ratio of the usage of catalyst to trimethoxy silane is 1*10<-6>-0.10, and the mass ratio of the usage of cocatalyst to trimethoxy silane is 5*10<-6>-0.10; 2) heating up to 0-150 DEG C under stirring, then continuously introducing ethylene for reaction; 3) stopping the reaction when the pressure in the reaction kettle is not decreased to obtain the synthetic product of ethyl trimethoxy silane; and 4) carrying out separation and extraction on the synthetic product to obtain ethyl trimethoxy silane.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a preparation method of ethyltrimethoxysilane, an intermediate commonly used in the preparation of resins, crosslinking agents and coupling agents. technical background [0002] Ethyltrimethoxysilane is an important organosilicon chemical reagent, which can be used as a crosslinking agent in the preparation of silicone rubber, as a raw material in the preparation of silicone resin, and as a silane coupling agent. It has important applications in the preparation of dielectric materials and insulating materials. [0003] At present, ethyltrimethoxysilane is mainly prepared by hydrosilylation process of trimethoxysilane and ethylene or hydrogenation process of vinyltrimethoxysilane and hydrogen, and its chemical reaction equations are as formula (1) and formula ( 2) as shown. [0004] HSi(OCH 3 ) 3 +CH 2 =CH 2 →C 2 h 5 Si(OCH 2 ) 3 (1) [0005] CH 2 =CHSi(OCH ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18B01J27/13
Inventor 来国桥董红刘玲伍川杨雄发彭家建厉嘉云白赢蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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