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A kind of preparation method of peroxide vulcanizable fluororubber

A technology of peroxide and fluororubber, applied in the field of peroxide vulcanizable fluororubber and its preparation, can solve the problems of small molecular weight of rubber, high price, few monomers at the vulcanization point, etc., so as to improve the permanent compression deformation performance. Effect

Active Publication Date: 2017-01-04
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Suspension polymerization is initiated by an oil-soluble initiator, and the resulting elastomer has no terminal ions and no emulsifier residues, but the molecular weight of the resulting rubber is relatively small
[0007] In addition, there are few researches on vulcanization point monomers in China, and they mainly rely on imports, which are not easy to source and expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 Peroxide vulcanized fluororubber and preparation method thereof

[0028] 1) In a 5L stainless steel reaction kettle with a stirrer, add 3L deionized water, 2g dipotassium hydrogen phosphate, 2g emulsifier (a mixture of perfluoropolyether ammonium carboxylate and sodium octyl sulfonate in equal weight ratios) , Repeated nitrogen pressurization, evacuation and degassing until the oxygen content ≤ 30ppm, the temperature of the reaction kettle was raised until the temperature inside the kettle was stabilized at 80°C.

[0029] 2) Add the mixed monomer of VDF / HFP=60 / 40 (molar ratio) to the reactor with a compressor until the pressure of the reactor reaches 1.5MPa, add 40g of vinyl bromide, and then press into 20g of 15% (wt) aqueous solution of ammonium persulfate, initiate polymerization reaction; When the pressure of the reactor drops to 1.4MPa, add ICH 2 CH 2 1.5g, add the mixed monomer of VDF / HFP=80 / 20 (mol ratio) simultaneously, keep the pressure in the re...

Embodiment 2

[0032] Embodiment 2 peroxide vulcanized fluororubber and preparation method thereof

[0033] 1) In a 5L stainless steel reaction kettle with a stirrer, add 3L deionized water, 2g dipotassium hydrogen phosphate, 2g emulsifier (a mixture of perfluoropolyether ammonium carboxylate and sodium octyl sulfonate in equal weight ratios) , after repeated nitrogen pressurization and evacuation and degassing, until the oxygen content was ≤30ppm, the temperature of the reactor was raised to 80°C.

[0034] 2) Use a compressor to add a mixed monomer of VDF / HFP=60 / 40 (molar ratio) to the reactor, increase the pressure to 1.5MPa, add 40g of 1,1-difluoro-2-bromoethylene, and pressurize through a metering pump Go into the 15% (wt) ammonium persulfate aqueous solution of 20g, initiate polyreaction, when reactor pressure drops to 1.4MPa, add iodoform 8g and add the mixed monomer of VDF / HFP=80 / 20 (mol ratio) simultaneously, Keep the pressure in the reactor at 1.5MPa.

[0035] 3) As the reaction p...

Embodiment 3

[0037] Embodiment 3 peroxide vulcanized fluororubber and preparation method thereof

[0038] 1) In a 5L stainless steel reaction kettle with a stirrer, add 3L deionized water, 2g dipotassium hydrogen phosphate, 2g emulsifier (a mixture of perfluoropolyether ammonium carboxylate and sodium octyl sulfonate in equal weight ratios) , repeated nitrogen pressurization, evacuation and degassing, and the temperature in the reaction kettle was raised to 80°C.

[0039]2) Use a compressor to add VDF / HFP / TFE=30 / 40 / 30 (molar ratio) mixed monomers into the reaction kettle until the pressure inside the kettle reaches 1.8MPa, add 20g of acrylonitrile, and then press in 10g of it through a metering pump 15% (wt) ammonium persulfate aqueous solution, trigger polymerization reaction, when the reactor pressure drops to 1.7MPa, add 4g methyl iodide and add the mixing unit of VDF / HFP / TFE=60 / 22 / 18 (mol ratio) simultaneously Body, keep the pressure in the reactor at 1.8MPa.

[0040] 3) As the react...

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Abstract

The invention provides a preparation method of fluororubber capable of being vulcanized by peroxide. The method comprises the following steps: 1) adding deionized water, a pH buffer agent and an emulsifier to a reaction kettle, carrying out vacuum supply operation on the reaction kettle, and heating the inside of the kettle to 50-120 DEG C; 2) adding a polymeric monomer A and a polymeric monomer B to the reaction kettle until the pressure in the kettle reaches 0.3-5MPa, adding a radical initiator to initialize polymerization reaction, adding a chain transfer agent after reaction is begun, simultaneously supplementing the polymeric monomer A and the polymeric monomer B, so as to maintain the pressure at the pressure in the kettle; 3) supplementing the radical initiator once at an interval of 4 hours along with reaction until the reaction is ended; and 4) obtaining an elastomer emulsion, adding a flocculant, condensing, washing and drying in vacuum, so as to obtain the fluororubber capable of being vulcanized by the peroxide. The fluororubber product vulcanized by the peroxide provided by the invention can be vulcanized by the peroxide, so that the permanent compression deformation resistance after hot air ageing is greatly improved.

Description

technical field [0001] The invention belongs to the field of macromolecular materials, and in particular relates to a peroxide-vulcanizable fluorine rubber and a preparation method thereof. Background technique [0002] Fluoroelastomers are widely used in products such as sealing materials, containers and hoses due to their excellent heat resistance, oil resistance and chemical resistance. The common peroxide-cured fluoroelastomers mainly include vinylidene fluoride as the main comonomer and tetrafluoroethylene as the main comonomer. Such as vinylidene fluoride (VDF), perfluoropropylene (HFP), tetrafluoroethylene (TFE), brominated olefin copolymer elastomer. [0003] In order to expand the physical properties of fluoroelastomers, the obtained fluoroelastomers must be cross-linked before they can be used. Its vulcanization system is a mixture of organic peroxides and multifunctional unsaturated coagents. Whereas the cross-link is located at the "I" or "Br" atom of the "C-I...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F214/22C08F214/28C08F214/26C08F214/16C08F214/18C08F220/44C08F220/50C08F2/38C08F2/26C08C1/15
Inventor 曾波张建新李斌白鲸兰军赵媛媛余金龙王先荣龚蓉
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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