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A kind of preparation method of ethyltrimethoxysilane

The technology of ethyltrimethoxysilane and trimethoxysilane is applied in the field of preparation of ethyltrimethoxysilane and can solve the problems of increasing rectification load, increasing investment cost of rectifying tower equipment, increasing operating cost of separation process and the like , to achieve the effect of improving selectivity and improving conversion rate

Active Publication Date: 2020-06-05
HENAN UNIVERSITY +1
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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

[0034] A kind of preparation method of ethyltrimethoxysilane, its step is: in the 2000mL synthetic still that is equipped with agitator, ethylene gas inserting tube, thermometer bushing, add raw material trimethoxysilane quality to be 353g, catalyst RuCl 3 ·xH 2 The quality of O is 0.0069g; after stirring at room temperature for 15min, feed 0.35MPa ethylene gas into the synthesis kettle from the gas insertion tube, and close the inlet valve; 2The mass of O is 0.0554g, feed 0.35MPa ethylene gas, keep the reaction temperature at 20-40°C and stir the reaction, close the ethylene inlet valve; when the pressure in the synthesis kettle no longer decreases, stop the reaction, and lower the contents in the kettle to room temperature collect.

[0035] The sample was 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 was 96.73%, tetramethoxysila...

Embodiment 2

[0037] A kind of preparation method of ethyltrimethoxysilane, its step is: in the 2000mL synthetic still that is equipped with agitator, ethylene gas inserting tube, thermometer bushing, add raw material trimethoxysilane quality to be 306g, catalyst RuCl 3 ·xH 2 The quality of O is 0.0201g; after stirring at room temperature for 15min, feed 0.35MPa ethylene gas into the synthesis kettle from the gas insertion tube, and close the inlet valve; 2 The mass of O is 0.0465g, feed 0.35MPa ethylene gas, keep the reaction temperature at 35-45°C and stir the reaction, close the ethylene inlet valve; when the pressure in the synthesis kettle no longer decreases, stop the reaction, and lower the contents of the kettle to room temperature collect.

[0038] The sample was 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 was 96.53%, tetramethoxysil...

Embodiment 3

[0040] A kind of preparation method of ethyltrimethoxysilane, its step is: in the 2000mL synthetic kettle that is equipped with agitator, ethylene gas insertion bottom tube, thermometer sleeve pipe, add raw material trimethoxysilane quality to be 288g, catalyst quality is RuCl 3 ·xH 2 The quality of O is 0.0370g; after stirring at room temperature for 15min, feed 0.35MPa ethylene gas into the synthesis kettle from the gas insertion tube, and close the inlet valve; 2 The mass of O is 0.0264g, feed 0.35MPa ethylene gas, keep the reaction temperature at 45-55°C and stir the reaction, close the ethylene inlet valve; when the pressure in the synthesis kettle no longer decreases, stop the reaction, and lower the contents in the kettle to room temperature collect.

[0041] The sample was 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 was ...

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Abstract

The invention provides a preparation method of ethyltrimethoxysilane. The preparation method comprises the following steps: adding trimethoxysilane, crystalline hydrate (RuCl3*xH2O) of ruthenium trichloride and a co-catalyst H2O into a pressure-resisting reaction kettle; controlling the temperature to be 20 to 70 DEG C and introducing ethylene to react; when the pressure in a reaction system is not changed any more, stopping reaction to obtain a synthetic product with the ethyltrimethoxysilane content which is greater than 94 percent and an ethyltrimethoxysilane and tetramethoxysilane mass concentration ratio coefficient beta which is greater than or equal to 52. The ethyltrimethoxysilane and the ethylene are used as raw materials, the cheap ruthenium trichloride crystalline hydrate is used as a catalyst and the water is used as the co-catalyst; any additional solvent is not needed; the ethyltrimethoxysilane is directly synthesized through hydrosilylation reaction; in the preparation method, the catalyst is low in price and small in dosage; reaction conditions are moderate and easy to control; the ethyltrimethoxysilane has high content and is easy to separate from a byproduct tetramethoxysilane with an approximate boiling point by adopting a rectification manner, so that the ethyltrimethoxysilane with high purity is obtained.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a preparation method of ethyl trimethoxy silicon. Background technique [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 3 ) 3 (1) [0005] CH 2 =CHSi(OCH 3 ) 3 +H 2 →C 2 h 5 Si(OCH 3 ) 3 (2) [0006] Russian Journal of General Chemistry (2006, 76(2): 22...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
CPCC07F7/1876
Inventor 刘玲伍川李景华刘蕾李习莹晏妍吕金伟贾海燕
Owner HENAN UNIVERSITY