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Preparation method of phenyl silicone resin

A technology of phenyl silicone resin and hydrocarbyl alkoxy silane is applied in the field of preparation of phenyl silicone resin, and can solve the problems of unguaranteed insulation stability and high temperature resistance of phenyl silicone resin.

Active Publication Date: 2010-11-03
东莞市贝特利新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There is a common problem in the above preparation methods of phenyl silicone resin: a large amount of organic solvents are used, and salt impurities that may have an important impact on the dielectric properties are brought in
The insulation stability and high temperature resistance of this phenyl silicone resin are not guaranteed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 63g of ethyl orthosilicate, 146g of phenyltriethoxysilane, 34g of methylphenyldimethoxysilane, 5g of dimethyldiethoxysilane and 20g of tetramethyldisiloxane into 500ml In a four-neck flask, heat and stir for 10 minutes, add 1.7 g of concentrated hydrochloric acid, and then add 72 g of ultrapure water dropwise, and the dropping time is controlled at about 25 minutes. React at a constant temperature of 40°C for 3h, then raise the temperature to 90°C to remove low boilers. Then add 490g of ultrapure water, reflux at 80°C for 2 hours, cool, layer and separate, pour out the water layer, then add 490g of ultrapure water as residual resin, reflux at 80°C for 2h, cool, layer and separate, pour out the water layer, This was repeated three times, and the water layer was poured out, and the low boilers were removed under vacuum at 180°C, and after decolorization and filtration by activated carbon, a colorless, transparent and uniform phenyl hydrogen-containing silicone resin w...

Embodiment 2

[0030] 100g phenyltrimethoxysilane, 30g vinyltrimethoxysilane, 45g methyl orthosilicate, 24.3g diphenyldimethoxysilane, 10g dimethyldiethoxysilane, 18g 1, Add 3-divinyltetramethyldisiloxane and 10g hexamethyldisiloxane into a 500ml four-neck flask, heat and stir for 10min, add 3g of concentrated sulfuric acid, then dropwise add 45g of ultrapure water, dropwise The time is controlled at about 25 minutes. React at a constant temperature of 50°C for 3h, then raise the temperature to 90°C to remove low boilers. Transfer the resin to a 1L three-necked bottle, add 400g of ultrapure water, reflux at 90°C for 2 hours, cool, layer and separate the liquid, pour out the water layer, then add 400g of ultrapure water for the residual resin, reflux at 90°C for 2 hours, then cool, separate Separate the layers, pour out the water layer, and repeat this 4 times, pour out the water layer, remove the low boilers in vacuum at 180°C, decolorize and filter with activated carbon, and obtain a color...

Embodiment 3

[0032] Add 220g of phenyltrimethoxysilane, 12g of methyl orthosilicate, 15g of dimethyldiethoxysilane and 30g of end-blocking 1,3-divinyltetramethyldisiloxane into a 500ml four-port In the bottle, heat and stir for 10 minutes, add 2.8 g of concentrated sulfuric acid, and then add 37 g of ultrapure water dropwise, and the dropping time is controlled at about 25 minutes. React at a constant temperature of 70°C for 3h, then raise the temperature to 95°C to remove low boilers. Transfer the resin to a 1L three-necked bottle, add 470g of ultrapure water, reflux at 90°C for 2 hours, cool, layer and separate the liquid, pour out the water layer, then add 470g of ultrapure water for the residual resin, reflux at 95°C for 2 hours, then cool, separate Separate the layers, pour out the water layer, and repeat this 4 times, pour out the water layer, remove the low boilers in vacuum at 180°C, decolorize and filter with activated carbon, and obtain a colorless, transparent and uniform phenyl...

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PUM

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Abstract

The invention relates to a preparation method of a phenyl silicone resin, which is used for preparing silicone resin free of solid salts by using alkyl alkoxy silane monomer and siloxane blocking agent as raw materials, using strong proton acid as a catalyst and cleaning and removing the catalyst with high-purity water at high temperature, wherein organic solvents are not used in the overall process. In the preparation process of the phenyl silicone resin of the invention, the strong proton acid is used as a hydrolytic condensation catalyst, and organic solvents are not used, thus the generating process is environment-friendly; and the catalyst is removed by rinsing, thus the prepared silicone resin is free of solid salt impurities.

Description

Technical field: [0001] The invention relates to the preparation of a silicone resin, in particular to a preparation method of a phenyl silicone resin. Background technique: [0002] Phenyl silicone resin is a silicone material with a special structure. In addition to the weather resistance, electrical insulation, waterproof, breathable and physiological inertia of ordinary silicone, this special material also has super high temperature and low temperature resistance. With high refractive index, it can be widely used as high-temperature-resistant paint and paint, and phenyl silicone resin without inorganic impurities has better high-temperature stability and electrical insulation, and can be used for the packaging of high-power light-emitting diodes. [0003] Patents US0116640A1 and US0032595A1 describe the use of chlorine-containing monomers to synthesize phenyl silicone resins that can be used for LED packaging by using an acid-base two-step method. In the patent CN101126...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/18
Inventor 王全苏俊柳奚家国李家忠
Owner 东莞市贝特利新材料有限公司
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