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Preparation method and application of trifluoroethyleneoxyphenyl-containing silicone resin

A technology of trifluorovinyloxyphenyl and dimethoxysilane, which is applied in the field of high-performance polymer manufacturing and can solve problems such as decreased adhesion

Inactive Publication Date: 2015-03-25
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has been reported that the developed silicone materials still have certain limitations. For example, the refractive index of methyl silicone resin is about 1.43, and the refractive index of methylphenyl silicone resin is 1.50. With the increase of phenyl content, The rigidity of the material is also increased accordingly, and the adhesion is reduced

Method used

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  • Preparation method and application of trifluoroethyleneoxyphenyl-containing silicone resin
  • Preparation method and application of trifluoroethyleneoxyphenyl-containing silicone resin
  • Preparation method and application of trifluoroethyleneoxyphenyl-containing silicone resin

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preparation example Construction

[0108] Described organosilicon resin can be prepared by following preparation method:

[0109] In an inert solvent, carry out hydrolytic polymerization with an alkoxysilane monomer containing trifluorovinyloxyphenyl selected from the group (a) and an alkoxysilane monomer selected from the group (b) to obtain the following: The organosilicon resin shown in formula I; Described group (a) comprises: methyl (trifluorovinyloxyphenyl) dimethoxysilane, trifluorovinyloxyphenyl trimethoxysilane, methyl ( Trifluorovinyloxyphenyl)diethoxysilane, trifluorovinyloxyphenyltriethoxysilane, or combinations thereof; the group (b) includes: ethyl orthosilicate, phenyltrimethoxy phenylsilane, methylphenyldimethoxysilane, phenyltriethoxysilane, diphenyldimethoxysilane, trimethylethoxysilane, dodecyltrimethoxysilane, or combinations thereof .

[0110] The hydrolysis polymerization reaction is preferably carried out in the presence of an acidic catalyst and / or water; preferably, the acidic catalys...

Embodiment 1

[0135] Example 1 Preparation of organosilicon resin I containing trifluoroethyleneoxyphenyl

[0136] Add 50 milliliters of water, 50 milliliters of concentrated hydrochloric acid and 30 milliliters of toluene into a clean 500 milliliter three-necked bottle, and add 3.6 grams of tetraethyl orthosilicate, 30.0 grams of phenyltrimethoxysilane, A mixture of 17.0 grams of methylphenyldimethoxysilane, 9.8 grams of methyl (trifluorovinyloxyphenyl) dimethoxysilane, 10.2 grams of trifluorovinyloxyphenyltrimethoxysilane and 20 milliliters of toluene Solution, the reaction temperature is controlled below 20°C, continue to react for 3h after the dropwise addition, then heat to 80°C for 3h, cool to room temperature, wash with water until neutral, dry the organic layer with anhydrous sodium sulfate, remove toluene after filtration , under reduced pressure and heated to 150° C. / 10 mba to remove small molecule compounds, and obtain 17.1 g of trifluoroethyleneoxyphenyl-containing organosilicon...

Embodiment 2

[0137] Example 2 Preparation of organosilicon resin II containing trifluoroethyleneoxyphenyl

[0138] Add 20 milliliters of water, 50 milliliters of acetic acid and 30 milliliters of toluene into a clean 500 milliliter three-necked bottle, and add 3.8 grams of orthosilicate, 41.3 grams of phenyltriethoxysilane, A mixture of 18.5 grams of methylphenyldimethoxysilane, 9.2 grams of methyl (trifluorovinyloxyphenyl) dimethoxysilane, 10.5 grams of trifluorovinyloxyphenyltrimethoxysilane and 20 milliliters of toluene Solution, the reaction temperature is controlled below 20°C, after the dropwise addition, heat to 100°C to continue the reaction for 16 h, cool to room temperature, wash with water until neutral, dry the organic layer with anhydrous sodium sulfate, remove toluene after filtration, and raise the temperature under reduced pressure Remove the small molecular compound at 150°C / 10mba to obtain 19.3 g of organosilicon resin II containing trifluoroethyleneoxyphenyl.

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Abstract

The invention provides a preparation method and application of trifluoroethyleneoxyphenyl-containing silicone resin. In the process of preparing the organic silicone resin, a trifluoroethyleneoxyphenyl-containing alkoxy silane monomer and various alkoxy silane monomers are hydrolyzed to be subjected to copolymerization to obtain the novel high-temperature cured silicone resin with a high refractive index, good heat resistance and excellent dielectric properties. The silicone resin can be applied to the fields of microelectronic industry, electrical appliances and aerospace as a high-performance resin matrix or packaging material.

Description

technical field [0001] The invention belongs to the field of high-performance polymer production, and in particular relates to a production method and application of a high-temperature-cured organic silicon resin material containing trifluoroethyleneoxyphenyl. Background technique [0002] In the development of science and technology, the development of construction, automation, electrical appliances, microelectronics, aerospace and other fields has an increasing demand for new materials, especially high-performance polymer materials, such as adhesives in the high-temperature field, which can be scaled down High-performance low-dielectric materials, composite materials, etc. for electronic components. In the field of microelectronics industry, the manufacture of 65nm chips based on copper interconnection technology urgently needs heat-resistant materials with low dielectric constant. Commonly used polyimide materials have good thermal stability and mechanical properties, but...

Claims

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Application Information

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IPC IPC(8): C08G77/24C08L83/08
Inventor 房强金凯凯
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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