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Nano emulsion of peroxide vulcanized fluororubber and polymerization method thereof

A peroxide and nanoemulsion technology, applied in the field of nanoemulsion and its polymerization, can solve the problems of reduced equipment utilization, affected production efficiency, low solid content, etc., to improve cold resistance, excellent mechanical properties and processing performance, increase The effect of flexibility

Inactive Publication Date: 2014-04-09
江苏梅兰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] CN101274969B has described a kind of microemulsion polymerization method of fluorine-containing polymer, and it adopts perfluorooctanoic acid ammonium or perfluorononanoic acid ammonium as emulsifier, and non-fluorine alkanol is co-emulsifier, and the microemulsion solid content of gained is lower than 10%, Therefore, the utilization rate of the equipment is greatly reduced, which affects the production efficiency.

Method used

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  • Nano emulsion of peroxide vulcanized fluororubber and polymerization method thereof

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Effect test

Embodiment 1

[0048] Add 6kg deionized, 60g fluoroether emulsifier (C 2 f 5 [OCF 2 CF(CF 3 )] 3 OCF 2 COONH 4 ), 3g of disodium hydrogen phosphate, 10g of molecular structure with a molecular weight of 600 are (1) co-emulsifier, open the steam regulating valve, heat up the deionized water in the reactor to 80°C, feed high-purity nitrogen and vacuumize the reaction The oxygen content in the kettle is replaced to ≤30ppm. Then, under the pressure of 3.5 MPa, 45% of vinylidene fluoride, 5% of tetrafluoroethylene and 50% of perfluoromethyl vinyl ether were mixed by a compressor. Add mass fraction and be 10% potassium persulfate solution 300g, initiate polymerization reaction, polymerization pressure drops, add mixed monomer again, mass fraction is 55% vinylidene fluoride, mass fraction is 10% tetrafluoroethylene, mass fraction 35% perfluoromethyl vinyl ether is pressed into the reaction kettle through a compressor, and the pressure and temperature are maintained for reaction. After react...

Embodiment 2

[0050] In the 20L reactor, add 12kg deionization, 130g fluoroether emulsifier (C 2 f 5 [OCF 2 CF(CF 3 )] 3 OCF 2 COONH 4 ), 6g of disodium hydrogen phosphate, 20g of molecular structure with a molecular weight of 600 are (1) co-emulsifier, open the steam regulating valve, heat up the deionized water in the reactor to 80°C, feed high-purity nitrogen and vacuumize the reaction The oxygen content in the kettle is replaced to ≤30ppm. Then, under the pressure of 3.5 MPa, 45% of vinylidene fluoride, 5% of tetrafluoroethylene and 50% of perfluoromethyl vinyl ether were mixed by a compressor. Add mass fraction and be 10% potassium persulfate solution 600g, initiate polymerization reaction, polymerization pressure drops, add mixed monomer again, mass fraction is 55% vinylidene fluoride, mass fraction is 10% tetrafluoroethylene, mass fraction 35% perfluoromethyl vinyl ether is pressed into the reaction kettle through a compressor, and the pressure and temperature are maintained f...

Embodiment 3

[0052] Add 30kg deionization, 300g fluoroether emulsifier (C 2 f 5 [OCF 2 CF(CF 3 )] 3 OCF 2 COONH 4 ), 15g of disodium hydrogen phosphate, 50g of molecular structure with a molecular weight of 600 are (1) co-emulsifier, open the steam regulating valve, heat up the deionized water in the reactor to 80°C, feed high-purity nitrogen and vacuumize the reaction The oxygen content in the kettle is replaced to ≤30ppm. Then, under the pressure of 3.5 MPa, 45% of vinylidene fluoride, 5% of tetrafluoroethylene and 50% of perfluoromethyl vinyl ether were mixed by a compressor. Adding mass fraction is 1500g of 10% potassium persulfate solution, initiates polymerization reaction, and polymerization pressure drops, adds mixed monomer again, and mass fraction is 55% vinylidene fluoride, mass fraction is 10% tetrafluoroethylene, mass fraction 35% perfluoromethyl vinyl ether is pressed into the reaction kettle through a compressor, and the pressure and temperature are maintained for rea...

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Abstract

The invention discloses a production method of a peroxide vulcanized fluoroelastomer, which comprises the following steps: 1. preparing three fluorine-containing monomer gases, a dispersant, a peroxide vulcanization point monomer, an initiator, a chain-transfer agent, a pH regulator and deionized water; 2. regulating pH value of a dispersion solution mixed from the deionized water, dispersant solution, initiator, chain-transfer agent and pH regulator, evacuating, replacing with nitrogen until the oxygen content is acceptable, and pouring the dispersion solution into a polymerization kettle; 3. collecting the three fluorine-containing monomer gases to a pressostat to keep the pressures of the three gases constant in the pressostat; 4. respectively passing the three fluorine-containing monomer gases through an adjusting valve and a mass flowmeter, evenly mixing in a static mixer, compressing to reaction pressure by a molding press, and sending into the polymerization kettle; 5. adding the peroxide vulcanization point monomer into a measuring pump; and 6. adding the peroxide vulcanization point monomer into the polymerization kettle to perform polymerization reaction with the three fluorine-containing monomer gases in the dispersion solution.

Description

technical field [0001] The invention relates to a nanoemulsion of peroxide vulcanized fluorine rubber and a polymerization method thereof. Background technique [0002] Fluoropolymers refer to high polymers with fluorine atoms attached to carbon atoms. Fluoropolymer materials are heat-resistant, oil-resistant, solvent-resistant, corrosion-resistant, strong oxidant-resistant and have good physical and mechanical properties. They are widely used in many fields such as aerospace, military industry, national defense, automobile, petroleum and chemical industry. [0003] Currently, the most commonly used methods for preparing fluoropolymers include suspension polymerization and emulsion polymerization. In the aqueous emulsion polymerization method, the polymerization reaction is carried out in the presence of perfluorinated emulsifiers. The commonly used emulsifiers PFOS (perfluorooctanesulfonyl compound) and PFOA (perfluorooctanoic acid ammonium) are highly stable and difficult...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F216/14C08F214/22C08F214/26C08F214/18C08F2/26C08F2/30C08F2/38C08F4/30
Inventor 代生华吴玉勋钱厚琴
Owner 江苏梅兰化工有限公司
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