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A kind of high vinyl active fluorosilicone rubber raw rubber and preparation method thereof

A fluorosilicone rubber and high vinyl technology, applied in the field of high vinyl active fluorosilicone rubber and its preparation, can solve the problem of insufficient vinyl activity and utilization rate, influence of processability and mechanical properties, and inability to achieve good cross-linking effect and other problems, so as to avoid low utilization rate, simple and effective preparation method, and reduce shielding effect.

Active Publication Date: 2022-07-15
新元化学(山东)股份有限公司 +1
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  • Summary
  • 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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  • A kind of high vinyl active fluorosilicone rubber raw rubber and preparation method thereof
  • A kind of high vinyl active fluorosilicone rubber raw rubber and preparation method thereof
  • A kind of high vinyl active fluorosilicone rubber raw rubber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] The preparation of vinyl fluorosilicon monomer includes steps as follows:

[0066] (1) under nitrogen protection, add 926g trifluoropropyl trichlorosilane and 1389g ethyl acetate in the reactor equipped with mechanical stirring, thermometer, condenser, constant pressure dropping funnel, open stirring and mix the materials, The temperature of the kettle was lowered to 0~10°C by an ice-water bath, and then the mixture of 470g vinyldimethylsilanol (purity 95.6%) and 445g triethylamine was added dropwise in the kettle to carry out dechlorination reaction, the reaction was exothermic, and the dropwise addition During this period, the temperature of the kettle was maintained at 0-10°C, and after the dropwise addition was completed, stirring was continued for 1-2 hours, then the system was returned to room temperature, and triethylamine hydrochloride was removed by filtration. The filter cake was washed with 200 g of ethyl acetate, and the filtrate was collected to obtain 1-eth...

Embodiment 2

[0070] The preparation of vinyl fluorosilicon monomer includes steps as follows:

[0071] (1) under nitrogen protection, add 833g trifluoropropyl trichlorosilane and 1200g ethyl acetate in the reactor equipped with mechanical stirring, thermometer, condenser tube, constant pressure dropping funnel, open stirring and mix the materials, The temperature of the kettle was lowered to 0~10°C by an ice-water bath, and then the mixture of 423g vinyldimethylsilanol (purity 95.6%) and 400g triethylamine was added dropwise to the kettle for dechlorination, the reaction was exothermic, and the dropwise addition During this period, the temperature of the kettle was maintained at 0-10°C, and after the dropwise addition was completed, stirring was continued for 1-2 hours, then the system was returned to room temperature, and triethylamine hydrochloride was removed by filtration. The filter cake was washed with 200 g of ethyl acetate, and the filtrate was collected to obtain 1-ethylene. yl-3-...

Embodiment 3

[0074] A kind of high vinyl active fluorosilicone rubber raw rubber has the following structure:

[0075]

[0076] The preparation steps are as follows:

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

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

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

[0080] (4) Under the pressure of -0.099MPa to -0.1MPa, the temperature is raised to 200-220°C, the small m...

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Abstract

The invention discloses a high vinyl active fluorosilicone rubber raw rubber and a preparation method thereof. In the molecular structure of the fluorosilicone rubber raw rubber, there is a dimethyl silicon oxide between the side chain vinyl group and the main chain silicon oxygen chain link. Compared with the form in which the pendant vinyl group is directly connected to the main chain silicon atom in the conventional fluorosilicone rubber raw rubber structure, this structure reduces the steric hindrance effect of the trifluoropropyl group and makes the vinyl group protrude from the silicon atom. In addition to the oxygen main chain, the reactivity of the vinyl group is greatly improved, and the vinyl fluorosilicon monomer of the present invention is compatible with D 3 F has good compatibility, close ring-opening activity, consistent polymerization rate, good copolymerization effect and high product yield.

Description

technical field [0001] The invention relates to the technical field of rubber materials, in particular to a high vinyl active fluorosilicone rubber raw rubber and a preparation method thereof. Background technique [0002] Fluorosilicone rubber raw rubber is a fluorosilicone 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 retardant and low surface energy of fluorine materials. It is an indispensable and important material in the fields of defense industry, aerospace, automobile industry and petrochemical industry. [0003] The vulcanization of fluorosilicone rubber takes the vinyl group in the molecular structure of the raw rubber as ...

Claims

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Application Information

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Patent Type & Authority Patents(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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