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Preparation method of alkali-proof vulcanized fluororubber

A technology for vulcanizing fluorine rubber and fluorine rubber, which is applied in the field of preparation of organic polymer materials and can solve problems such as difficulty in carrying out

Active Publication Date: 2013-12-11
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent US 4148982 discloses a copolymer of tetrafluoroethylene and propylene to obtain unsaturated double bonds by heat treatment, and then vulcanized by peroxide, but this process is difficult to carry out

Method used

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  • Preparation method of alkali-proof vulcanized fluororubber

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Experimental program
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Effect test

Embodiment 1

[0049] Batch free radical emulsion polymerization was carried out in a 50L autoclave to prepare fluororubber. Add 30L deionized water and 100g 5wt% ammonium perfluorooctanoate aqueous solution in the reactor, 20g pH regulator disodium hydrogen phosphate, the air in the vapor space in the reactor is first replaced with nitrogen, and then replaced with mixed monomers, so that the oxygen content is less than 20ppm, the temperature of the reactor was raised to 120°C. The polymerized monomer mixture was added into the reactor with a diaphragm compressor to raise the pressure to 3.5 MPa. After reaching 3.5MPa, the reactor pressure controller is set to automatically operate at 3.5MPa. The polymerized monomer is composed of 45% vinylidene fluoride, 25% hexafluoropropylene and 22.5% tetrafluoroethylene, 1.5% vulcanization point monomer BVE, 6% monomer CH 2 =CH-CH 3 Composition, the total weight is 12Kg.

[0050] When the pressure of the reactor reaches 3.5MPa, start stirring, fully...

Embodiment 2

[0055]Batch free radical emulsion polymerization was carried out in a 50L autoclave to prepare fluororubber. Add 30L deionized water and 100g 4wt% perfluorooctanoic acid ammonium aqueous solution in reactor, 20g pH adjusting agent borax, the air in steam space in reactor is replaced with nitrogen earlier, then with mixed monomer replacement, make oxygen content less than 25ppm, will The temperature of the reactor was raised to 110°C. Add the polymerization monomer mixture into the reaction kettle with a diaphragm compressor to raise the pressure to 3.5Mpa. After reaching 3.5Mpa, the reactor pressure controller is set at 3.5MPa for automatic operation. The polymerized monomer is composed of 37% vinylidene fluoride, 15% chlorotrifluoroethylene and 22.5% tetrafluoroethylene by mole, and 1.5% vulcanization point monomer CF 2 = CFBr, 3% CH 2 =CH-CH 2 CH 3 , with a total weight of 12Kg.

[0056] When the pressure of the reactor reaches 4.5MPa, start stirring, fully mix the mix...

Embodiment 3

[0060] Batch free radical emulsion polymerization was carried out in a 50L autoclave to prepare fluororubber. Add 30L deionized water and 100g 6wt% ammonium perfluorooctanoate aqueous solution in the reactor, 20g pH adjuster dipotassium hydrogen phosphate, the air in the vapor space in the reactor is first replaced with nitrogen, and then replaced with mixed monomers, so that the oxygen content is less than 25ppm, the temperature of the reactor was raised to 70°C. The polymerized monomer mixture was added into the reactor with a diaphragm compressor to raise the pressure to 2.5 MPa. After reaching 3.5MPa, the reactor pressure controller is set to automatically operate at 3.5MPa. The polymerized monomer is composed of 40% vinylidene fluoride, 25% perfluoropropyl vinyl ether (PPVE) and 23.5% tetrafluoroethylene by mole, and 1.5% vulcanization point monomer CF 2 =CFI, monomer CH 2 =CH-(CH 2 ) 3 -H 10%, the total weight is 12Kg.

[0061] When the pressure of the reactor reac...

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Abstract

The invention provides a preparation method of alkali-proof vulcanized fluororubber. The preparation method includes steps of (1), adding water, emulsifiers and pH (potential of hydrogen) modifiers in a reactor; (2), adding polymerized monomers; (3), starting a stirring device, increasing temperature to be 70-120 DEG C, and adding initiators and chain transfer agents so as to start polymerization reaction; (4), adding residual polymerized monomers in batches, and stopping reaction after all the polymerized monomers are added so as to obtain polymerized emulsion; (5), coagulating, washing and drying the polymerized emulsion to obtain fluororubber; and (6), vulcanizing the fluororubber obtained in the step (5) so as to obtain the vulcanized fluororubber. The preparation method is simple in operation and requires mild reaction conditions. The structure of the fluororubber is controlled effectively by means of regulating structures of the monomers, changing reaction temperatures and the like, so that peroxide, namely the alkali-proof vulcanized fluororubber, is prepared. The prepared vulcanized fluororubber with high Mooney viscosity also has good curability and good oil resistance and can be applied to various industrial fields.

Description

technical field [0001] The invention belongs to the field of preparation of organic polymer materials, and in particular relates to a preparation method of alkali-resistant vulcanized fluororubber. Background technique [0002] Fluorine rubber (fluororubber) refers to a synthetic polymer elastomer containing fluorine atoms on the carbon atoms of the main chain or side chain. The earliest fluorine rubber was poly-2-fluoro-1.3-butadiene and its copolymers with styrene and propylene, which were trial-produced by DuPont Company of the United States in 1948, but its performance was not better than that of chloroprene rubber and butyl rubber. Expensive, no real industrial value. In the late 1950s, Thiokol Company of the United States developed a kind of low-temperature performance, strong resistance to strong oxidants (N 2 o 4 ) of binary nitrosofluororubber, fluororubber began to enter practical industrial applications. Since then, with the advancement of technology, various ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/24C08L27/16C08K5/14C08F214/22C08F214/28C08F214/26C08F214/24C08F216/14
Inventor 兰军张建新李斌高家勇白鲸赵少春余金龙王先荣
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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