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A kind of preparation method of fluorine rubber raw rubber

A technology of fluororubber raw rubber and compound dispersant, which is applied in the field of fluororubber synthesis, can solve the problems of complicated process, low density of fluororubber raw rubber, heat resistance and poor liquid resistance of vulcanized rubber, and achieves simple process and product performance. Good, solvent-resistant performance

Active Publication Date: 2021-10-12
ZHEJIANG JUSHENG FLUOROCHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fluorine rubber generally uses common amine or polyol vulcanizing agents as vulcanizing agents. However, common amine or polyol vulcanizing agents for high fluorine-containing rubber with a raw rubber specific gravity above 1.9 are extremely difficult to vulcanize, or the product performance after vulcanization is not ideal.
[0003] Chinese Patent Publication No. CN108102259A discloses a preparation method of bisphenol vulcanized fluororubber. The obtained elastomer has low compression set and good resilience, but due to the vulcanization characteristics of bisphenol system, the tensile strength of the vulcanized rubber is low.
[0004] Chinese Patent Publication No. CN106832691A discloses a peroxide-cured fluororubber synthesized from a monomer mixture of VDF, HFP, and 1.1-difluoro-2-bromoethylene in a molar ratio of 65:30:5. The vulcanized composition is water-resistant The steam performance is good, but the fluorine content of raw rubber is low, the solvent resistance and oil resistance are poor, and it cannot be used in demanding fields
However, the fluororubber raw rubber obtained by this method has a low density, and the heat resistance and liquid resistance of the vulcanized rubber are poor, and the process is cumbersome and the production time is too long, which is not conducive to realizing efficient industrial production

Method used

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  • A kind of preparation method of fluorine rubber raw rubber
  • A kind of preparation method of fluorine rubber raw rubber

Examples

Experimental program
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Effect test

Embodiment 1

[0034] (1) In a steel kettle equipped with a stirrer, at a speed of 15000r / min, 900g C 8 f 15 NaO 2 and 180gCH 3 O(C 2 h 4 O) 3 H stirs 0.1h, obtains composite dispersant microemulsion, for subsequent use;

[0035] (2) In a 50L stainless steel horizontal reactor, add 25kg of high-purity water, remove nitrogen and oxygen until the oxygen content is less than or equal to 10ppm, add the composite dispersant microemulsion obtained in 60g step (1), 30g disodium hydrogen phosphate, 30g4-iodine -3,3,4,4-tetrafluorobutene, stirred at 40rpm for 10min;

[0036] (3) Heat the reactor to 70°C at a stirring speed of 40rpm, add a mixed monomer of vinylidene fluoride, tetrafluoroethylene and perfluoropropylene with a molar ratio of 30:50:20 until the pressure of the reactor is 3.0MPa, and pass nitrogen Add 20g of ammonium persulfate into the reaction kettle to start the polymerization reaction. During the reaction, the compressor is continuously used to add the mixed monomer of vinylid...

Embodiment 2

[0039] (1) In a steel kettle equipped with a stirrer, at a speed of 17000r / min, mix 800g C 8 h 4 f 15 NO 2 and 200gCH 3 OCH 2 CH 2 OH was stirred for 0.3h to obtain a composite dispersant microemulsion for subsequent use;

[0040] (2) In a 50L stainless steel horizontal reactor, add 25kg of high-purity water, remove nitrogen and oxygen until the oxygen content is less than or equal to 10ppm, add 65g of the composite dispersant microemulsion obtained in step (1), 30g of disodium hydrogen phosphate, and 32g of difluoro Vinyl bromide, stirred at 50rpm for 20min;

[0041] (3) Heat the reactor to 80°C at a stirring speed of 50rpm, add a mixed monomer of vinylidene fluoride, tetrafluoroethylene and perfluoropropylene with a molar ratio of 45:30:25 until the pressure of the reactor is 1.5MPa, and pass nitrogen Add 20g of ammonium persulfate into the reaction kettle to start the polymerization reaction. During the reaction, the compressor is continuously used to add the mixed m...

Embodiment 3

[0044] (1) In a steel kettle equipped with a stirrer, at a speed of 10000r / min, 700g C 8 f 15 NaO 2 and 280gCH 3 O(C 2 h 4 O) 3 H stirs 0.5h, obtains composite dispersant microemulsion, for subsequent use;

[0045] (2) In the 50L stainless steel horizontal reactor, add 27kg of high-purity water, remove nitrogen and deoxygenate until oxygen content is less than or equal to 10ppm, add the composite dispersant microemulsion that 72g step (1) obtains, 40g disodium hydrogen phosphate, 40g 4- Bromo-3,3,4,4-tetrafluorobutene, stirred at 60rpm for 5min;

[0046] (3) Heat the reactor to 90°C at a stirring speed of 60rpm, add a mixed monomer of vinylidene fluoride, tetrafluoroethylene and perfluoropropylene with a molar ratio of 36:47:17 until the pressure of the reactor is 1.5MPa, and pass nitrogen Add 50g of ammonium persulfate into the reaction kettle to start the polymerization reaction. During the reaction, the compressor is continuously used to add the mixed monomer of viny...

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Abstract

The invention discloses a preparation method of fluorine rubber raw rubber, which comprises mixing fluorine-containing carbon carboxylate and ethylene glycol monomethyl ether to obtain a composite dispersant microemulsion; and then mixing high-purity water, a pH regulator, Put the composite dispersant microemulsion and vulcanization point monomer into the reactor for stirring; then raise the temperature of the reactor to 50-100°C, add polymerized monomers into the reactor until the pressure inside the reactor is 1-5 MPa, add the initiator 20-50 During the reaction process, the reaction pressure is maintained constant by adding polymerized monomers, and when the conversion rate of the polymerized monomers is 30-40%, 30-50 parts of chain transfer agents are added; finally, when the reaction liquid-solid content reaches 20 ~40%, the reaction is finished, and the obtained polymer emulsion is washed and dried after electrolyte coagulation to obtain a fluororubber raw rubber product. The present invention has the advantages of simple process, excellent solvent resistance, fuel oil resistance and chemical resistance of the product .

Description

technical field [0001] The invention relates to the field of fluororubber synthesis, in particular to a preparation method of fluororubber raw rubber. Background technique [0002] Fluororubber sulfide has excellent properties such as heat resistance, solvent resistance, weather resistance and ozone resistance, and is widely used in sealing materials such as oil seals, packings, gaskets, O-rings, diaphragms, hoses and linings, coating bonding and other industrial fields . However, with the emergence of new environmentally friendly energy sources and fuels, there are higher requirements for the performance of fluorine rubber in solvent resistance and chemicals. Early studies have proved that the erosive effect of alcoholic gasoline on rubber materials is much stronger than that of pure gasoline, and the erosive effect of methanol-containing gasoline on rubber is much greater than that of ethanol-containing gasoline. Among all kinds of rubber, the alcohol-resistant gasoline ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F214/26C08F214/18C08F214/22C08F214/28
CPCC08F214/182C08F214/22C08F214/26C08F214/28
Inventor 程宇汤阳余考明陈伟峰朱洪吉陈佳王鑫黄群益叶智萍任慧芳
Owner ZHEJIANG JUSHENG FLUOROCHEM