Synthetic method of 2-cyanoethyl triethoxysilane

A technology of cyanoethyltriethoxysilane and cyanoethyltrichlorosilane is applied in the field of synthesis of 2-cyanoethyltriethoxysilane and can solve the problems of poor demoulding, surface scratches and poor luster. and other problems, to achieve the effect of inhibiting side reactions, improving product quality and yield

Inactive Publication Date: 2016-05-11
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, acrylonitrile copolymer plastics also have many shortcomings, such as surface scratches, poor luster, cracks and whitening, uneven color, fragility, and poor mold release, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Put 377g of 2-cyanoethyl trichlorosilane and 480g of polybasic acid diethyl ester into a 2000ml three-necked flask with magnetic stirring and slowly raise the temperature to 60°C-120°C, then start stirring at a stirring speed of 20-100 rpm, and keep constant Add 230g of absolute ethanol into the funnel, and start dropping when the temperature rises to 70°C, and the dropping time is controlled within 2 hours;

[0021] After the dropwise addition, 467g of dehydrated ethanol was added to the constant pressure funnel of the decompression reaction distillation device, and when the vacuum degree of decompression remained at -0.03MPa~-0.05MPa, dehydrated ethanol was added dropwise, and the reaction temperature rose slowly to 130°C, aging for 1h after feeding;

[0022] The aged crude product is subjected to rectification and purification, the temperature is controlled at: 120°C-140°C, the temperature at the top of the rectification tower is controlled at 100°C-110°C, and the va...

Embodiment 2

[0024] Put 377g of 2-cyanoethyl trichlorosilane and 480g of polybasic acid diethyl ester into a 2000ml three-necked flask with magnetic stirring and slowly raise the temperature to 60°C-120°C, then start stirring at a stirring speed of 20-100 rpm, and keep constant Add 230g of absolute ethanol into the funnel, and start dropping when the temperature rises to 70°C, and the dropping time is controlled within 2 hours;

[0025] After the dropwise addition, add 467g of dehydrated ethanol into the constant pressure funnel of the decompression reaction distillation device. ℃, aging for 1h after feeding;

[0026] The aged crude product is subjected to rectification and purification, the temperature is controlled at: 120°C-140°C, the temperature at the top of the rectification tower is controlled at 100°C-110°C, and the vacuum degree of decompression is controlled at: -0.08MPa~-0.1MPa to obtain its The product is 398g of colorless transparent liquid, product testing results: main cont...

Embodiment 3

[0028] Put 377g of 2-cyanoethyl trichlorosilane and 480g of polybasic acid diethyl ester into a 2000ml three-necked flask with magnetic stirring and slowly raise the temperature to 60°C-120°C, then start stirring at a stirring speed of 20-100 rpm, and keep constant Add 230g of absolute ethanol into the funnel, and start dropping when the temperature rises to 70°C, and the dropping time is controlled within 2 hours;

[0029] After the dropwise addition, add 467g of dehydrated ethanol into the constant pressure funnel of the decompression reaction distillation device. ℃, aging for 1h after feeding;

[0030] The aged crude product is subjected to rectification and purification, the temperature is controlled at: 120°C-140°C, the temperature at the top of the rectification tower is controlled at 100°C-110°C, and the vacuum degree of decompression is controlled at: -0.08MPa~-0.1MPa to obtain its The product is 410g of colorless transparent liquid, product testing results: main cont...

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PUM

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Abstract

The invention relates to a synthetic method of 2-cyanoethyl triethoxysilane, which belongs to the technical field of fine chemicals. The synthetic method comprises the following steps: dropwise adding absolute ethyl alcohol into a three-opening flask esterification device filled with 2-cyanoethyl trichlorosilane by virtue of a constant-pressure funnel, performing the synthetic reaction, wherein the molar ratio of the 2-cyanoethyl trichlorosilane to the absolute ethyl alcohol is 1: (2.5 to 2.8), adding a catalyst (acid diethyl ester) into the three-opening flask before the reaction, controlling the reaction temperature at 60 to 120 DEG C, controlling the dropwise adding time at 2h to 4h, performing secondary esterification for an esterified crude product, re-filling the constant-pressure funnel with 3mol of absolute ethyl alcohol under a decompressing condition (-0.03MPa to -0.05MPa), recycling the surplus absolute ethyl alcohol by adopting a distilling recycling device, and decompressing and distilling a crude product after the secondary esterification is completed to obtain a colorless transparent product, wherein the content can be controlled to be 99 percent or more, and cl is less than or equal to 5ppm.

Description

technical field [0001] The invention relates to a synthesis method of 2-cyanoethyltriethoxysilane, which belongs to the technical field of fine chemicals. Background technique [0002] 2-cyanoethyltriethoxysilane is a new type of silane coupling agent used in glass fiber reinforced plastics, plastics, casting and other industries in recent years. Acrylonitrile copolymer plastics have a strong ability to bear loads. Adding glass fiber additives can increase the strength and thermal deformation resistance and reduce the thermal expansion coefficient. Therefore, it is widely used in electrical appliances, daily commodities, automobile industry, household products, cosmetics product packaging etc. However, acrylonitrile copolymer plastics also have many shortcomings, such as surface scratches, poor luster, cracks and whitening, uneven color, fragility, and poor mold release. Contents of the invention [0003] The object of the invention is to: provide a kind of synthetic met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C07F7/20
CPCC07F7/1804C07F7/188C07F7/20
Inventor 吴兵兵刘明锋陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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