Method for preparing fluorine silicon rubber base glue

A technology of fluorosilicone rubber and base rubber, which is applied in the field of preparation of fluorosilicone rubber base rubber for the automotive industry and aerospace industry, and can solve the problems of fluorosilicone rubber tear strength, mechanical strength, high temperature aging, and oil resistance. , to achieve the effect of excellent mechanical properties and excellent oil resistance

Inactive Publication Date: 2008-05-14
广东信力特种橡胶制品有限公司
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Problems solved by technology

[0012] The tear strength, mechanical strength, high temperature aging, and oil resistance of the fluorosilicone rubber obtained by the above preparation methods are difficult to have at the same time.

Method used

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  • Method for preparing fluorine silicon rubber base glue

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preparation example Construction

[0041]The preparation of fluorosilicone additives adopts the ring-opening polycondensation method. Mix and dehydrate hydroxyfluorosilicone oil, fluorosilicone monomer D3F, and vinyl monomer at 50-100°C for 1-3 hours, then add silanol sodium salt, and then mix and dehydrate for 0.2 ~1 hour. Raise the temperature to 115-150°C to react for 0.5-6 hours, then cool down to 60-90°C, add an equal volume of ethyl acetate and stir to dissolve, then wash with water until the pH value is close to 7, and finally evaporate the solvent to obtain the required fluorosilicone Agent, determination of viscosity, vinyl content, hydroxyl value.

[0042] The material needs to be mixed and dehydrated before reacting, and the dehydration condition is -0.01~-0.02MPa. The material can be dehydrated and added to the reactor, or dehydrated in the reactor.

[0043] It is required to control the hydroxyl value of the fluorosilicone additive to 1-6%, and the molar content of vinyl units to be 5-50%.

[00...

example 1

[0050] Add 100 grams of fluorosilicone monomer D3F monomer, 100 grams of hydroxyl fluorosilicone oil (hydroxyl value 6%), 50 grams of vinyl silicon monomer, and 0.8 grams of silanol sodium salt into a pre-dried 1000 ml reaction kettle. Turn on stirring, control the temperature at 70±3°C, -0.01~0.02MPa, pass in dry nitrogen, and dehydrate for 3 hours; then raise the temperature to 125°C±3°C, pass in dry nitrogen during the reaction process, and cool the system to 60°C after 25 minutes ℃, add 250 g of ethyl acetate and stir to dissolve. The material is washed with water until neutral, and the solvent is evaporated to obtain the desired fluorosilicone additive. The vinyl content and hydroxyl value in the fluorine-containing silicon additives were tested by chemical titration. The hydroxyl value of the fluorosilicone additive is 2.2%, and the molar content of vinyl units is 31%;

example 2

[0052] Change the quality of the vinyl silicon monomer to 10 grams, and other conditions are the same as in example 1. The hydroxyl value of the obtained fluorosilicone additive is 2.8%, and the molar content of vinyl units is 11% respectively;

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Abstract

The invention relates to a preparation method of fluorosilicone rubber base rubber, providing a preparation method of hydroxyl end capped fluorine silicon promoter with fluorine silicon structural unit and ethylene unit and certain polymerization degree, for preparing fluorosilicone rubber base rubber with excellent mechanical properties, high temperature properties and oil resistant properties. The invention prepares fluorine silicon promoter materials, materials of fluorine silicon promoter adopting open loop condensational procedure via general fluorine silicon monomer, vinyl silicone monomer, basic promoter and regulator, and obtains the needed fluorine silicon promoter; the fluorine silicon promoter and other promoters are added in the fluorine silicon raw rubber; the fluorine silicon raw rubber, the fluorine silicon promoter and the tetra butyl peroxy hexane are mixed uniformly for 5 to 60 minutes on a open mill or a internal mixer, thefluorosilicone rubber base rubber can be obtained after discharging. The invention prepares excellent fluorosilicone rubber base rubber with excellent mechanical properties, high temperature properties and oil resistant properties.

Description

technical field [0001] The invention relates to a preparation method of a fluorosilicone rubber base rubber, in particular to a preparation method of a fluorosilicone rubber base rubber used in automobile industry and aerospace industry. Background technique [0002] Fluorosilicone rubber is a special synthetic rubber material whose main chain is a silicon-oxygen-containing structure and the side chain is a fluorine-containing alkyl structure. The special chemical structure of this material makes it not only have the excellent high and low temperature performance of silicone rubber, but also have the excellent high temperature resistance, chemical medium resistance and oil resistance of fluororubber. The fluorosilicone rubber here mainly refers to heat vulcanized fluorosilicone rubber. The structure of raw fluorosilicone rubber is as follows: [0003] [0004] In the structure of raw fluorosilicone rubber, the vinyl unit acts as a vulcanization point, while the excellen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/24C08G77/20C08G77/06C08L83/07C08K5/01
Inventor 郑日土
Owner 广东信力特种橡胶制品有限公司
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