Raw fluorosilicone rubber with high vinyl activity and preparation method thereof

A fluorosilicone rubber and high vinyl technology, which is applied in the field of high vinyl active fluorosilicone rubber and its preparation, can solve the problems of processing performance, mechanical properties, insufficient vinyl activity and utilization rate, and inability to achieve good cross-linking effect and other problems, to achieve the effect of simple and effective preparation method, avoiding low utilization rate and reducing shielding effect

Active Publication Date: 2021-05-07
新元化学(山东)股份有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, no matter which method is used in the prior art to prepare raw fluorosilicone rubber, the vinyl group in its molecular structure is directly connected to the silicon atom of the main chain, and appears in the form of vinyl methyl silicone chain link
Due to the large steric hindrance effect of the trifluoropropyl group, the raw rubber structure will have a certain shielding effect on the adjacent silicon vinyl group, resulting in a decrease in the reactivity of the vinyl group in the raw rubber molecular chain, and the vinyl genes gather in the One part of the molecular chain cannot exert the cross-linking effect of each vinyl group. During the vulcanization process, due to insufficient vinyl activity and utilization, it is often impossible to achieve a good cross-linking effect, resulting in incomplete vulcanization of fluorosilicone rubber. The product is soft and sticky, poor in strength, including processing performance and mechanical properties, etc. are affected to a certain extent

Method used

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  • Raw fluorosilicone rubber with high vinyl activity and preparation method thereof
  • Raw fluorosilicone rubber with high vinyl activity and preparation method thereof
  • Raw fluorosilicone rubber with high vinyl activity and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] The preparation of vinyl fluorine silicon monomer comprises steps as follows:

[0066] (1) Under nitrogen protection, add 926g trifluoropropyl trichlorosilane and 1389g ethyl acetate to the reactor equipped with mechanical stirring, thermometer, condenser, constant pressure dropping funnel, start stirring and mix the materials evenly, Use an ice-water bath to lower the temperature of the kettle to 0-10°C, then dropwise add a mixture of 470g of vinyldimethylsilanol (purity 95.6%) and 445g of triethylamine to the kettle for dechlorination reaction, the reaction is exothermic, dropwise During this period, keep the temperature of the kettle at 0-10°C, continue stirring for 1h-2h after the dropwise addition is completed, then return the system to room temperature, remove triethylamine hydrochloride by filtration, wash the filter cake with 200g of ethyl acetate, collect the filtrate, and obtain 1-ethylene Base-3-trifluoropropyl-1,1-dimethyl-3,3-dichlorodisiloxane solution;

...

Embodiment 2

[0070] The preparation of vinyl fluorine silicon monomer comprises steps as follows:

[0071] (1) Under the protection of nitrogen, add 833g trifluoropropyltrichlorosilane and 1200g ethyl acetate to the reaction kettle equipped with mechanical stirring, thermometer, condenser, constant pressure dropping funnel, start stirring and mix the materials evenly, Use an ice-water bath to lower the temperature of the kettle to 0-10°C, then dropwise add a mixture of 423g vinyldimethylsilanol (95.6% purity) and 400g triethylamine to the kettle for dechlorination reaction, the reaction exothermic, dropwise During this period, keep the temperature of the kettle at 0-10°C, continue stirring for 1h-2h after the dropwise addition is completed, then return the system to room temperature, remove triethylamine hydrochloride by filtration, wash the filter cake with 200g of ethyl acetate, collect the filtrate, and obtain 1-ethylene Base-3-trifluoropropyl-1,1-dimethyl-3,3-dichlorodisiloxane solutio...

Embodiment 3

[0074] A high vinyl active fluorosilicone rubber raw rubber with the following structure:

[0075]

[0076] The preparation steps are as follows:

[0077] (1) Add 5200g trimethyltri(3,3,3-trifluoropropyl)cyclotrisiloxane (D 3 F) and 56g of vinyl fluorosilicon monomer of formula (II), start stirring, and dehydrate under the conditions of 40°C to 50°C and -0.099MPa to -0.1MPa for 2h;

[0078] (2) Use high-purity nitrogen to restore the pressure, then add 30g vinyl dimethyl silanol (purity 95.6%) and 4.3g sodium hydroxide alkali gel (NaOH content 4.02%) to the kettle and slowly heat up to 120°C for copolymerization Reaction, after the reaction starts, keep stirring at 120°C to 130°C for 3h;

[0079] (3) After the reaction is complete, add 90g of vinyldimethylacetoxysilane into the kettle, keep stirring at 100°C to 120°C for 12h for neutralization and capping;

[0080] (4) Under the pressure of -0.099MPa to -0.1MPa, raise the temperature to 200-220°C, remove small molecules ...

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PUM

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Abstract

The invention discloses a raw fluorosilicone rubber with high vinyl activity and a preparation method thereof, in the molecular structure of the raw fluorosilicone rubber, a dimethyl silica chain link exists between a side chain vinyl and a main chain silica chain link, and compared with the form that the side group vinyl is directly connected to a main chain silicon atom in the conventional raw fluorosilicone rubber structure, the steric hindrance effect of trifluoropropyl is reduced, vinyl protrudes out of a silicon-oxygen main chain, the reaction activity of vinyl is greatly improved, the vinyl fluorosilicone monomer has good compatibility with D3F, the ring opening activity is close, the polymerization rate is consistent, the copolymerization effect is good, and the product yield is high.

Description

technical field [0001] The invention relates to the technical field of rubber materials, in particular to a high-vinyl active fluorosilicone raw rubber and a preparation method thereof. Background technique [0002] Fluorosilicone rubber raw rubber is a fluorosiloxane polymer with a silicon-oxygen bond as the main chain and trifluoropropyl and methyl groups as side groups. It maintains the heat resistance, cold resistance, electrical insulation, and resistance of silicone materials. On the basis of excellent properties such as aging, it also has a series of performance characteristics such as excellent hydrocarbon solvent resistance, oil resistance, flame retardancy, and low surface energy of fluorine materials. It can be used to prepare oil-resistant parts for various locomotives, aircrafts, and petrochemicals. , is an essential and important material in the fields of defense industry, aerospace, automobile industry and petrochemical industry. [0003] The vulcanization of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/24C08G77/20C08G77/08C08G77/38
CPCC08G77/24C08G77/20C08G77/08C08G77/38
Inventor 于鹏飞杜辉丛洋王华杰侯志伟夏子祥解乐福
Owner 新元化学(山东)股份有限公司
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