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Organic silicon perfusion resin and preparation method thereof

A silicone and resin technology, applied in the field of silicone resin and its preparation, can solve the problems of poor anti-halation performance, low heat resistance level, easy foaming due to heat release, etc.

Active Publication Date: 2012-03-21
ZHUZHOU TIMES ELECTRIC INSULATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of this invention is to relate to and propose a preparation method of silicone potting resin, which is proposed in view of the current potting resins that have low heat resistance level and shortcomings such as poor anti-halation performance, serious heat release and easy foaming during curing A silicone-based solvent-free infusion resin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0016] Take ethyl orthosilicate, dimethylvinylethoxysilane, methyldichlorosilane, and diphenyldichlorosilane monomers, and determine the ratio of the above raw materials according to the R / Si value of 1.0. In the flask, add water twice the total molar amount of the starting silane monomer raw material and toluene that is 1.0 times the starting silane monomer raw material, and add HCl gas adsorbent pyridine that is 1 times the total molar amount of the silane monomer raw material formula. Slowly add the organosilicon monomer dropwise to the flask with rapid stirring at a lower temperature of 5-20°C, drop the hydrolysis reaction for 3 hours, and then concentrate to separate the resin layer, at 80-120°C Reflux aging reaction for 2 hours, then wash and filter with water, remove the solvent used for hydrolysis under reduced pressure at 110-140°C, and regularly take samples to measure the viscosity of the resin, when the cone-plate viscosity of the product is 1500-3000CP (60°C) That...

example 2

[0018] Take vinyltrichlorosilane, trimethylchlorosilane, methyldichlorosilane, diphenyldichlorosilane, and phenyltrichlorosilane monomers, and the above-mentioned silane monomer raw materials are determined according to the R / Si value of 1.2. Ratio, add the water of 3.5 times of the starting silane monomer raw material molar total amount and be the xylene of 1.8 times of the starting silane monomer raw material total amount in the flask, add the HCl gas adsorbent hexamethanone of 2.0 times of the silane monomer raw material formula molar total amount base disilazane. Slowly add the organosilicon monomer dropwise to the flask with rapid stirring at a lower temperature of 5-20°C, drop the hydrolysis reaction for 4 hours, and then concentrate to separate the resin layer, at 80-120°C Reflux aging reaction for 4 hours, then wash and filter with water, remove the solvent used for hydrolysis under reduced pressure at 110-140°C, and take regular samples during the period to measure th...

example 3

[0020] Get monophenyltrichlorosilane, methylvinyldichlorosilane, dimethylchlorosilane, diphenyldichlorosilane, and dimethyldichlorosilane monomers, and the raw materials of the above-mentioned silane monomers are 1.3 according to the R / Si value Determine the proportion, add 5 times the water of the starting silane monomer raw material molar total amount and 3 times of the initial silane monomer raw material toluene and ethyl acetate in the flask, add 3 times the silane monomer raw material formula molar total amount of HCl Gas adsorbent triethanolamine. Slowly add the organosilicon monomer dropwise to the flask with rapid stirring at a lower temperature of 5-20°C, and the dropwise hydrolysis reaction lasts for 6 hours, and then concentrate to separate the resin layer, at 80-120°C Reflux aging reaction for 5 hours, then wash and filter with water, remove the solvent used for hydrolysis under reduced pressure at 110-140°C, and take samples regularly to measure the viscosity of t...

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PUM

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Abstract

The invention relates to organic silicon perfusion resin and a preparation method thereof. The preparation method comprises the following steps: selecting at least one silane monomer expressed according to a structure formula RnSiX4-n as an initial material, wherein R is an organic group and can be alkyl, aryl or vinyl, X is a hydrolysable group and can be chlorine atom, alkoxy or acyloxy, n is equal to 0 or 1 and the initial material comprises a vinylsilane monomer or hydrogen-containing silane monomer; determining the proportion of the initial material according to a silicon resin R / Si value of 1.0-1.3, dropwise adding the initial material into a flask adding with water, weak-polarity solvent and HCl gas absorbent at 5-20 DEG C, carrying out hydrolysis reaction for 3-6 h, concentrating,separating a resin layer, carrying out reflux curing reaction at 80-120 DEG C for 2-5 h, washing with water, filtering, removing solvent for hydrolysis by decompression at 110-140 DEG C, and discharging when the cone-plate viscosity of the product is 1,500-3,000 CP at 60 DEG C. The organic silicon perfusion resin has no rapid heat release, does not generate bubble in the curing process and has higher heat resistance and excellent corona resistant performance.

Description

technical field [0001] The present invention relates to a kind of organosilicon resin and its preparation method, especially to a kind of group containing Si-C=C and Si-H two kinds of structures, and its structure also contains at least the group consisting of R n SiX 4-n (wherein R is an organic group, which can be an alkyl group, an aryl group or a vinyl group; X is a hydrolyzable group, which can be a chlorine atom, an alkoxy group or an acyloxy group, etc.; n is 0 or 1) obtained by hydrolysis R n SiO (4-n) / 2 The silicone perfusion resin of the structural group and the preparation method thereof belong to the field of macromolecular polymerization. Background technique [0002] Potting resin is currently widely used in the filling and packaging of electronic components, semiconductors and integrated circuits, high-voltage power transmission and transformation equipment, electrical appliances and other fields. In one special functional material. Generally, the infusio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/12C08G77/06
Inventor 衷敬和李强军姜其斌陈子荣蔡彬芬
Owner ZHUZHOU TIMES ELECTRIC INSULATION