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Preparation method of epoxy silane oligomer

A technology of epoxy silane and oligomers, which is applied in the field of preparation of epoxy silane oligomers, can solve the problems of processing environmental pollution, product color darkening, affecting product content, etc., and achieves high purity, undiminished activity, and low volatile effect

Active Publication Date: 2017-05-17
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 3-(2,3-Glycidoxypropoxy)propylalkoxysilane is a widely used polymer work aid, widely used in plastics, coatings and adhesives to improve the mechanical strength of composite materials, Improve the electrical insulation performance of integrated circuit materials and printed circuit boards in wet state; in acrylic latex, polyurethane and two-component epoxy resin, the adhesion can be greatly improved, but the alkoxy group connected to silicon in the molecule will produce hydrolysis reaction, Lead to the formation of various by-products of lower alcohols that volatilize into the air, pollute the processing environment, and cause certain harm to the human body
[0006] Quaternary ammonium salts and organometallic compounds can also have a certain catalytic effect on the hydrolysis of alkoxysilanes, but these substances usually have good solubility in polymers, and are not easy to remove after the reaction, affecting product content and cause the product to darken in color

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 472 g of 3-(2,3-epoxypropoxy)propyltrimethoxysilane and 47 g of tert-butanol into a 1000ml four-necked flask equipped with mechanical stirring, a thermometer, a spherical condenser, and a constant pressure funnel, And start to stir and heat up. Weigh 0.054 g of sodium chloride with an analytical balance and dissolve it in 27 g of distilled water, transfer it to a constant pressure funnel and wait for dropwise addition. When the temperature of the solution in the flask was raised to 40°C, the sodium chloride solution was added dropwise, and the dropping speed was kept as uniform as possible, and the dropwise addition was completed within 2 h. During the dripping process, the solution in the flask will heat up due to the hydrolysis reaction, and appropriate cooling measures should be taken to keep the reaction temperature between 40-45°C. After the dropwise addition, continue to keep the temperature for aging reaction for 1 h. Then distill at normal pressure first, ...

Embodiment 2

[0025] Add 472 g of 3-(2,3-epoxypropoxy)propyltrimethoxysilane and 47 g of tert-butanol into a 1000ml four-necked flask equipped with mechanical stirring, a thermometer, a spherical condenser, and a constant pressure funnel, And start to stir and heat up. Weigh 0.054g of sodium carbonate dissolved in 27g of distilled water with an analytical balance, transfer to a constant pressure funnel and wait for dropwise addition. When the temperature of the solution in the flask was raised to 40°C, the sodium chloride solution was added dropwise, and the dropping speed was kept as uniform as possible, and the dropwise addition was completed within 2 h. During the dripping process, the solution in the flask will heat up due to the hydrolysis reaction, and appropriate cooling measures should be taken to keep the reaction temperature between 40-45°C. After the dropwise addition, continue to keep the temperature for aging reaction for 1 h. Then the temperature was raised to 95° C., and th...

Embodiment 3

[0026] Embodiment 3 does not use tert-butanol as solvent and compares with embodiment 1

[0027] Add 472 g of 3-(2,3-glycidoxy)propyltrimethoxysilane into a 1000ml four-neck flask equipped with a mechanical stirrer, a thermometer, a spherical condenser, and a constant pressure funnel, and start to stir and heat up. Dissolve 0.054 g of sodium chloride in 27 g of distilled water with an analytical balance, transfer to a constant pressure funnel and wait for dropwise addition. When the temperature of the solution in the flask was raised to 40°C, the sodium chloride solution was added dropwise, and the dropping speed was kept as uniform as possible, and the dropwise addition was completed within 2 h. During the dripping process, the solution in the flask will heat up due to the hydrolysis reaction, and appropriate cooling measures should be taken to keep the reaction temperature between 45-50°C. After the dropwise addition, continue to keep the temperature for aging reaction for ...

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Abstract

The invention relates to a preparation method of epoxy silane oligomer and belongs to the field of preparation of polymer organic materials. Epoxy silane and a solvent are added to a flask; after the flask is heated to 40-42 DEG C, a catalyst is dissolved in distilled water, the solution is slowly dropwise added by the aid of a constant-pressure funnel, the mixture reacts at the constant temperature for 0.8-1.2 h, the solvent and alcohol produced through hydrolysis are removed through heating under the normal pressure; a crude product of epoxy silane oligomer is obtained, filtration is performed with a conventional method for precipitation of the catalyst, and a finished product of epoxy silane oligomer is obtained. The prepared organopolysiloxane has the advantages of being colorless, transparent, high impurity, low in volatility, low in VOC emission, convenient to use, environment-friendly and the like. Meanwhile, the used catalyst can be separated through filtration after the reaction and can be reused without activity decrease.

Description

technical field [0001] The invention relates to a preparation method of epoxy silane oligomer, belonging to the field of preparation of high molecular organic materials. Background technique [0002] Organopolysiloxanes have important applications in organic-inorganic composite materials. Functional organopolysiloxanes containing epoxy groups can improve the surface activity, low-temperature flexibility and weather resistance of polymers. [0003] 3-(2,3-Glycidoxypropoxy)propylalkoxysilane is a widely used polymer work aid, widely used in plastics, coatings and adhesives to improve the mechanical strength of composite materials, Improve the electrical insulation performance of integrated circuit materials and printed circuit boards in wet state; in acrylic latex, polyurethane and two-component epoxy resin, the adhesion can be greatly improved, but the alkoxy group connected to silicon in the molecule will produce hydrolysis reaction, It leads to the generation of various by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C07F7/18
CPCC07F7/1804C07F7/1892C08G77/045
Inventor 靳军张宇陈圣云简永强甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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