High-activity hydrogen-containing fluorosilicone oil cross-linking agent and preparation method thereof

A technology of hydrofluorosilicone oil and crosslinking agent, which is applied in the field of rubber materials, can solve the problems of insufficient activity of silicon hydrogen, achieve good storage stability, high product yield, and improve mechanical properties

Active Publication Date: 2020-11-13
威海新元新材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the crosslinking agent, there is a dimethylsiloxane chain link between the methyl hydrogen siloxane chain link and the trifluoropropyl methylsiloxane chain link in the main chain, which can weaken the shie

Method used

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  • High-activity hydrogen-containing fluorosilicone oil cross-linking agent and preparation method thereof
  • High-activity hydrogen-containing fluorosilicone oil cross-linking agent and preparation method thereof
  • High-activity hydrogen-containing fluorosilicone oil cross-linking agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] A highly active hydrofluorosilicone oil crosslinking agent with the following structure:

[0055]

[0056] The preparation steps are as follows:

[0057] (1) Preparation of methyltrimethoxysilane hydrolyzate:

[0058] Add 680g of methyltrimethoxysilane and 7g of macroporous strongly acidic styrene-based cation exchange resin to a four-necked flask equipped with a mechanical stirrer, a thermometer, a reflux tube, and a dropping funnel, start stirring and mix evenly, and heat up to 50°C. Then, 72g of distilled water was added dropwise to the system for hydrolysis and condensation reaction. During the dropping process, the system released heat, and the addition rate was adjusted so that the temperature of the kettle did not exceed 60°C. After the dropwise addition was completed, the temperature was continued to rise to 67°C for reflux reaction and maintained for 5 hours;

[0059] After the reaction is complete, lower the system to room temperature, filter the resin, co...

Embodiment 2

[0066] A highly active hydrofluorosilicone oil crosslinking agent with the following structure:

[0067]

[0068] The preparation steps are as follows:

[0069] (1) Preparation of methyltrimethoxysilane hydrolyzate:

[0070] Add 408g of methyltrimethoxysilane and 8g of macroporous strongly acidic styrene-based cation exchange resin to a four-necked flask equipped with mechanical stirring, a thermometer, a reflux tube, and a dropping funnel, start stirring and mixing evenly, and heat up to 52°C. Then add 36g of distilled water dropwise to the system for hydrolysis and condensation reaction. During the dropwise addition, the system releases heat. Adjust the rate of addition so that the temperature of the kettle does not exceed 60°C. After the dropwise addition is completed, continue to heat up to 67°C for reflux reaction and maintain for 6h;

[0071] After the reaction is complete, lower the system to room temperature, filter the resin, collect the filtrate, and remove the m...

Embodiment 3

[0078] A highly active hydrofluorosilicone oil crosslinking agent with the following structure:

[0079]

[0080] The preparation steps are as follows:

[0081] (1) Preparation of methyltrimethoxysilane hydrolyzate:

[0082] Add 1088g of methyltrimethoxysilane and 16g of macroporous strongly acidic styrene-based cation exchange resin into a four-necked flask equipped with mechanical stirring, a thermometer, a reflux tube, and a dropping funnel, start stirring and mixing evenly, and heat up to 50°C. Then add 126g of distilled water dropwise to the system for hydrolysis and condensation reaction. During the dropwise addition, the system releases heat. Adjust the rate of addition so that the temperature of the kettle does not exceed 60°C. After the dropwise addition is completed, continue to heat up to 67°C for reflux reaction and maintain for 6h;

[0083] After the reaction is complete, lower the system to room temperature, filter the resin, collect the filtrate, and remove ...

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Abstract

The invention discloses a high-activity hydrogen-containing fluorosilicone oil cross-linking agent and a preparation method thereof. The molecular structure of the cross-linking agent is shown in thespecification, a dimethyl silicon-oxygen chain link exists between the side hydrogen and the main chain silicon-oxygen chain link; compared with a structure in which side group hydrogen in a conventional hydrogen-containing fluorosilicone oil structure is directly connected to a silicon atom of a main chain, according to the structure, the steric hindrance effect of trifluoropropyl is reduced, theshielding influence of trifluoropropyl on silicon hydrogen is reduced, the reaction activity of silicon hydrogen on a main chain is improved, a good vulcanization effect can be achieved by adding a small amount of additive fluorosilicone rubber in a vulcanization system of the additive fluorosilicone rubber, and the mechanical property of the fluorosilicone rubber is improved.

Description

technical field [0001] The invention relates to the technical field of rubber materials, in particular to a high-activity hydrofluorosilicone oil crosslinking agent and a preparation method thereof. Background technique [0002] The addition type of fluorosilicone rubber uses vinyl-containing polyfluorosiloxane as the base rubber, and silicon-hydrogen-containing oligosiloxane as the crosslinking agent. An elastic body that forms a three-dimensional network structure. Among them, the crosslinking agent of addition-type fluorosilicone rubber usually refers to hydrogen-containing fluorosilicone oil, the product viscosity ranges from 20 to 500 mPa.s, and the hydrogen content is between 0.01 and 1.6%. The structure of the crosslinking agent hydrofluorosilicone oil has a significant impact on the performance of fluorosilicone rubber, because the hydrofluorosilicone oil introduces part of the trifluoropropylmethylsiloxane into the main chain dimethyl silicone chain link The chain...

Claims

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Application Information

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IPC IPC(8): C08G77/24C08G77/12C08G77/08C08G77/06C08L83/08C08K7/26
CPCC08G77/24C08G77/12C08G77/08C08G77/06C08L83/08C08L2312/00C08L2205/025C08K7/26
Inventor 于鹏飞杜辉邵军强于佳平邹伟王华杰丛洋
Owner 威海新元新材料有限公司
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