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Environment-friendly high-temperature-resistant hybrid organic silicon resin with zirconium-doped main chain and preparation method thereof

A green and environmentally friendly silicone technology, applied in the field of green and high temperature resistant hybrid silicone resin and its preparation, to achieve the effects of improving heat resistance stability, excellent heat resistance and environmental friendliness

Inactive Publication Date: 2020-01-17
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, silicone resin decomposes initially at 360-400°C, but in the field of aerospace, materials need to be used for a long time above 1000°C, which is difficult to meet the wide application in aerospace industry, so the structure of silicone resin is modified to improve Its heat-resistant temperature urgently needs to be solved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In this example, phenyltriethoxysilane and methyltriethoxysilane are selected as T structural units for siloxane, methylphenyldiethoxysilane is used as D structural unit, and n-propanol is selected as organic zirconium source. Zirconium, chelating agent selects acetylacetone, carries out hydrolysis polycondensation reaction, forms the organosilicon resin containing Si-O-Zr structure (M n at 2700~3000).

[0023] The specific preparation method is as follows:

[0024] (1) 0.72mol of methyltriethoxysilane, 0.32mol of phenyltrimethoxysilane, 0.32mol of methylphenyldiethoxysilane and 60mL of absolute ethanol are packed into a three-necked flask, and 600rpm / min magnetic stirring, add 4.08mol deionized water drop by drop, the whole process temperature does not exceed 70°C, to obtain the mixed solution A;

[0025] (2) Dissolve 0.56mol of zirconium n-propoxide in 1.12mol of acetylacetone, stir evenly, and record it as mixed solution B;

[0026] (3) Gradually drop the mixed so...

Embodiment 2

[0032] In this example, methyltriethoxysilane is selected as the T structural unit for the siloxane, diphenyldiethoxysilane is used as the D structural unit, zirconium isopropoxide is selected as the organic zirconium source, and resorcinol is selected as the chelating agent. , carry out hydrolysis polycondensation reaction, and form the silicone resin containing Si-O-Zr structure (M n at 2550~2900).

[0033] The specific preparation method is as follows:

[0034] (1) Put 0.60mol of methyltriethoxysilane, 0.40mol of diphenyldiethoxysilane and 50mL of absolute ethanol into a three-necked flask, stir magnetically at 400rpm / min, and add 3.12mol of Deionized water, the temperature of the whole process does not exceed 70 ° C, to obtain the mixed solution A;

[0035] (2) Dissolve 0.16mol of zirconium isopropoxide in 0.32mol of resorcinol, stir evenly, and record it as mixed solution B;

[0036] (3) Gradually drop the mixed solution B into the mixed solution A. The temperature dur...

Embodiment 3

[0042] In this example, phenyltriethoxysilane is selected as the T structural unit for siloxane, dimethyldiethoxysilane is used as the D structural unit, zirconium n-propoxide is selected as the organic zirconium source, and resorcinol is selected as the chelating agent. , carry out hydrolysis polycondensation reaction, and form the silicone resin containing Si-O-Zr structure (M n at 2500~2800).

[0043] The specific preparation method is as follows:

[0044] (1) Put 0.48mol of phenyltriethoxysilane, 0.16mol of dimethyldiethoxysilane and 50mL of absolute ethanol into a three-necked flask, stir magnetically at 500rpm / min, and add 2.16mol of Deionized water, the temperature of the whole process does not exceed 70 ° C, to obtain the mixed solution A;

[0045] (2) Dissolve 0.15mol of zirconium n-propoxide in 0.30mol of resorcinol, stir evenly, and record it as mixed solution B;

[0046] (3) Gradually drop the mixed solution B into the mixed solution A. The temperature during th...

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PUM

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Abstract

The invention discloses an environment-friendly high-temperature-resistant hybrid organic silicon resin with a zirconium-doped main chain. The organic silicon resin is characterized in that the structural formula of the organic silicon resin is as follows: (R2SiO2 / 2) x (RSiO3 / 2) y (ZrO4 / 2) z (S) k, in the formula, R2SiO2 / 2, RSiO3 / 2 and ZrO4 / 2 respectively represent D unit siloxane, T unit siloxaneand an organic zirconium source; x, y, z and k respectively represent the number of structural units of R2SiO2 / 2, RSiO3 / 2, ZrO4 / 2 and S; R independently represents a methyl group or a phenyl group; Sis selected from one of siloxane groups, -Si (OH) 3, -RSi (OH) 2, -R2Si (OH), -R2SiOR, -RSiOR2 and-SiOR3, and ZO4 / 2 is selected from an organic zirconium source. By adopting a novel modified copolymerization mode, the resin material has better high temperature resistance than existing silicon resin material, and can be used as matrix resin for preparing a composite material and a high-temperature-resistant adhesive.

Description

technical field [0001] The invention relates to a silicone resin and a preparation method thereof, in particular to a green, environment-friendly and high-temperature-resistant hybrid silicone resin whose main chain is doped with zirconium and a preparation method thereof. Background technique [0002] Since its appearance in the 1940s, silicone resins have been widely used in electrical protective covers, transportation equipment, high temperature resistant adhesives, etc. Adhesives and other fields. [0003] Silicone resin is a highly cross-linked polysiloxane in structure, its main chain is Si-O-Si structure, in which the bond energy of Si-O bond is about 456kJ / mol, and the bond energy of Si-C bond is about The bond energy is 347kJ / mol, while in general organic resins, the bond energy of the C-C bond is about 332kJ / mol, so the Si-O bond structure in the silicone resin is not easy to be destroyed, and has excellent thermal stability. It has broad application prospects in...

Claims

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Application Information

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IPC IPC(8): C08G79/00C08G77/00
CPCC08G77/00C08G79/00
Inventor 刘丽姜警黄玉东
Owner HARBIN INST OF TECH
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