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A kind of preparation method of perfluoroether elastomer and obtained perfluoroether elastomer

A technology of elastomer and perfluoroether, which is applied in the field of preparation of fluoroelastomer to achieve the effect of increasing flexibility and enhancing crosslinking density

Active Publication Date: 2018-05-29
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

However, domestic enterprises have not yet occupied their due position in the field of perfluoroelastomers (2001, Liu Lingmei, "Overview of the Properties and Applications of Fluorine Rubber")

Method used

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  • A kind of preparation method of perfluoroether elastomer and obtained perfluoroether elastomer
  • A kind of preparation method of perfluoroether elastomer and obtained perfluoroether elastomer
  • A kind of preparation method of perfluoroether elastomer and obtained perfluoroether elastomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 5L stainless steel reaction kettle equipped with a stirrer, add 3L of deionized water, 2g of dipotassium hydrogen phosphate, 2g of emulsifier (a mixture of perfluoropolyether peroxide and sodium octyl sulfonate at a mass ratio of 1:1), After repeated nitrogen pressurization and evacuation and degassing, add a mixed monomer of TFE / PMVE / PPVE=60 / 35 / 5 (molar ratio) into the reactor with a compressor, raise the pressure to 1.2MPa at 80°C, and measure 10 g of perfluorobromoethyl vinyl ether and 10 g of 15% (wt) ammonium persulfate aqueous solution were pumped in to initiate polymerization. When the pressure of the reactor drops to 1.0MPa, add ICHF 2 CHF 2 1 5g, add the mixed monomer of VDF / HFP=80 / 20TFE / PMVE / PPVE=60 / 35 / 5 (mol ratio) simultaneously, keep the pressure in the reactor to be 1.2MPa.

[0032] As the reaction proceeds, add 10 g of initiator aqueous solution every 4 hours, that is, 15% (wt) ammonium persulfate aqueous solution once. The reaction continued for ...

Embodiment 2

[0039] In a 5L stainless steel reaction kettle with a stirrer, add 3L deionized water, 2g dipotassium hydrogen phosphate, 2g emulsifier (a mixture of perfluoropolyether peroxide and sodium octyl sulfonate at a mass ratio of 1:1), repeat After nitrogen pressurization and evacuation and degassing, add a mixed monomer of TFE / PMVE / PEVE=60 / 35 / 5 (molar ratio) into the reactor with a compressor, raise the pressure to 1.2MPa at 80°C, and pass through the metering pump 10 g of perfluorobromoethyl vinyl ether and 10 g of 15% (wt) ammonium persulfate aqueous solution were pressed in to initiate the polymerization reaction. When the pressure of the reactor drops to 1.0MPa, add I(CF 2 CF 2 ) 2 1 8g, add the mixed monomer of TFE / PMVE / PEVE=60 / 35 / 5 (mol ratio) simultaneously, keep the pressure in the reactor to be 1.2MPa.

[0040] As the reaction proceeds, 15% (wt) ammonium persulfate aqueous solution of 10 g of the initiator is added once every 4 h. The reaction continued for about 10 hour...

Embodiment 3

[0044] In a 5L stainless steel reaction kettle with a stirrer, add 3L of deionized water, 2g of dipotassium hydrogen phosphate, and 2g of emulsifier. After repeated nitrogen pressurization, evacuation and degassing, add TFE / PMVE / The mixed monomer of PEVE / PPVE=65 / 30 / 2 / 3 (molar ratio), boost to 1.2MPa at 80 ℃, press into 10g perfluorobromoethyl vinyl ether by metering pump, 15% of 10g ( wt) ammonium persulfate aqueous solution, initiate polymerization reaction, when the reactor pressure drops to 1.0MPa, add I(CF 2 ) 5 1 4g add the mixed monomer of TFE / PMVE / PEVE / PPVE=65 / 30 / 2 / 3 (molar ratio) simultaneously, keep the internal pressure of reactor to be 1.2MPa.

[0045] As the reaction proceeds, 15% (wt) ammonium persulfate aqueous solution of 10 g of the initiator is added once every 4 h. The reaction continued for about 8 hours, and about 4.5kg of elastomer emulsion was obtained. Coagulate with sodium chloride aqueous solution, wash, and continue drying in a vacuum oven at 80°C...

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Abstract

The invention discloses a preparation method of a perfluoroether elastomer. The preparation method comprises the step of carrying out emulsion polymerization on four comonomers in the presence of an initiator and a chain transfer agent, so as to prepare a fluorine-containing elastomer, wherein the four comonomers are as follows: the first monomer is tetrafluoroethylene, the second monomer is perfluoromethyl vinyl ether, the third monomer is a vulcanization point monomer, and the fourth monomer is pentafluoroethyl vinyl ether and / or pentafluoropropyl vinyl ether; and the fluorine-containing elastomer is prepared from the following steps: adding water into a reaction container, introducing a mixture of the first monomer, the second monomer and the fourth monomer, maintaining the pressure of the container at 0.5MPa-2.0MPa, adding 2g / L-10g / L of the third monomer according to the mass volume ratio, and carrying out polymerization reaction. According to the preparation method, the monomers such as PEVE / PPVE are used in the reaction, so that the rigidity of molecular chains can be reduced, the flexibility of molecular chains can be increased, and the hardness of the perfluoroether elastomer is reduced.

Description

technical field [0001] The invention relates to the field of fluorine-containing elastomers, in particular to a preparation method of peroxide-curable fluorine-containing elastomers. Background technique [0002] Fluorine rubber has been widely used in various fields, but with the continuous advancement of science and technology, the human demand for special fluoroelastomers is getting higher and higher. Such as low-temperature-resistant fluororubber, solvent-resistant fluororubber, and 300°C high-temperature-resistant fluororubber. Perfluororubber mainly consists of tetrafluoroethylene and perfluoroalkyl vinyl ether as the main monomers, and uses cyano-containing perfluoroolefins and (perfluoro)phenoxyolefins as vulcanization point monomers for copolymerization, as shown in its name In that way, the hydrogen atoms on all carbon atoms in the polymer are replaced by fluorine atoms, and have an extremely stable structure to high temperature and chemicals, such as the high tem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F214/26C08F216/14C08F2/38C08F2/26C08F2/30C08L27/18
Inventor 曾波汪仲权张建新李斌王先荣余金龙张廷健龚蓉
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD