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Fluorosilicone resin and preparation method thereof

A technology of fluorosilicone resin and pentafluorophenylethyl dimethyl chlorosilane, which is applied in the field of high-temperature resistant fluorosilicone resin and its preparation, can solve problems such as insufficient heat resistance, achieve superior heat resistance, and avoid excessive exchange Combined, the effect of high yield

Active Publication Date: 2018-09-04
SHENZHEN TAIKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the shortcoming of insufficient heat resistance existing in the existing silicone resin, and provides a new silicone resin and its preparation method

Method used

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  • Fluorosilicone resin and preparation method thereof
  • Fluorosilicone resin and preparation method thereof
  • Fluorosilicone resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Synthesis of pentafluorophenethyldimethylchlorosilane

[0042]500mL three-neck flask, equipped with thermometer, reflux condenser and constant pressure dropping funnel, heated by oil bath. Add 80 g of toluene and 65 g of pentafluorostyrene in sequence, stir and dissolve, and add 0.26 g of chloroplatinic acid catalyst under nitrogen protection. Turn on the heating, and after the temperature rises to 80° C., 51 g of methyldichlorohydrosilane is added dropwise, and the dropping time is controlled at about 1 hour. After the dropwise addition, the insulation reaction was continued for 2 hours. After the reaction, the solvent and unreacted methyldichlorosilane were distilled off, and the 132°C fraction (3.75kPa) was collected by distillation under reduced pressure to obtain 95g of pentafluorophenethyldimethylchlorosilane. The purity of the product measured by gas chromatography was 96.6 %, yield 90.9%.

[0043] (2) Condensation to synthesize fluorosilicone resin

[00...

Embodiment 2

[0053] (1) The synthesis process of pentafluorophenethyldimethylchlorosilane is the same as in Example 1.

[0054] (2) Condensation to synthesize fluorosilicone resin

[0055] In a 250mL Erlenmeyer flask, 19.4g of pentafluorophenethyldimethylchlorosilane, 5.5g of trimethylmonochlorosilane and 63g of ethyl orthosilicate were uniformly mixed to obtain a mixed silane, which was set aside.

[0056] 500mL three-neck flask, equipped with thermometer, reflux condenser and constant pressure dropping funnel, heated by oil bath. First carefully and slowly pour 8g of water and 5g of concentrated sulfuric acid into 50g of tetrahydrofuran, heat the mixture to 70°C, then add the pre-prepared mixed silane dropwise, and the dropping time is controlled at about 42min. After the addition, the reaction was incubated for 6 hours.

[0057] The reaction was stopped, and the reaction solution was distilled under reduced pressure to remove the by-product ethanol and the solvent tetrahydrofuran. The...

Embodiment 3

[0062] (1) Synthesis of pentafluorophenethyldimethylchlorosilane

[0063] 500mL three-neck flask, equipped with thermometer, reflux condenser and constant pressure dropping funnel, heated by oil bath. Add 40 g of trifluoromethylbenzene and 32 g of pentafluorostyrene in sequence, stir and dissolve, and add 0.1 g of chloroplatinic acid catalyst under nitrogen protection. Turn on the heating, and after the temperature rises to 80°C, add 26g of methyldichlorohydrosilane dropwise, and the dropping time is controlled at about 1 hour. After the dropwise addition, the insulation reaction was continued for 1.5 hours. After the reaction, the solvent and unreacted methyldichlorosilane were distilled off, and the 132°C fraction (3.75kPa) was collected by distillation under reduced pressure to obtain 46g of pentafluorophenethyldimethylchlorosilane. The purity of the product measured by gas chromatography was 95.8 %, yield 84.6%.

[0064] (2) Polycondensation synthesis of pentafluorophen...

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Abstract

The invention discloses fluorosilicone resin and a preparation method thereof. The method comprises the following steps: pentafluorostyrene is used as a raw material, and pentafluorophenethyldimethylchlorosilane is obtained by a hydrosilylation reaction; and the pentafluorophenethyldimethylchlorosilane, trimethylchlorosilane and ethyl orthosilicate are subjected to a polycondensation reaction to prepare the pentafluorophenyl silicon resin. When the resin disclosed by the invention is prepared, a secondary polycondensation process is adopted, so that the defect of a larger difference of hydrolysis reactivity of the pentafluorophenethyldimethylchlorosilane and copolymerized trialkylmonochlorosilane is overcome, and a preparation yield is high; the obtained pentafluorophenyl silicone resin has superior heat resistance; the method has the advantages of a simple preparation process, low requirements on equipment and raw materials easy to obtain, and is suitable for industrialized enlarged production; and the heat-resistant fluorosilicone resin can be applied to high-molecular materials such as heat-resistant adhesives.

Description

technical field [0001] The invention relates to a high-temperature-resistant fluorosilicone resin and a preparation method thereof. The produced product can be used as a polymer modification or a polymer additive, and belongs to the field of organosilicon synthesis and polymer additives. Background technique [0002] Silicone resin is a kind of thermosetting plastic, one of its most prominent properties is excellent thermo-oxidative stability and excellent electrical insulation performance, it can maintain its good insulation performance in a wide range of temperature and frequency. Silicone resin is usually made of various mixtures of methyltrichlorosilane, dimethyldichlorosilane, phenyltrichlorosilane, diphenyldichlorosilane or methylphenyldichlorosilane in the presence of organic solvents such as toluene , Decomposed by adding water at a lower temperature to obtain an acidic hydrolyzate. The initial products of hydrolysis are a mixture of cyclic, linear and crosslinked p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/24C08G77/20C08G77/12C08G77/06C08L83/08
CPCC08G77/06C08G77/12C08G77/20C08G77/24C08L83/08C08L2201/08
Inventor 李战雄纵亚坤李武龙
Owner SHENZHEN TAIKE TECH
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