Fluorine and chlorine-containing conducting polymer resin preparation method

A conductive polymer and resin technology, applied in the field of preparation of fluorine-containing and chlorine-containing conductive polymer resins, can solve problems such as functional decline, poor creep resistance, and deformation of membrane structure, and achieve high mechanical strength, excellent physical and chemical properties. performance effect

Active Publication Date: 2017-07-14
ZHEJIANG HYPROOF TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Fluorine-containing conductive polymers such as DuPont's Nafion resin have excellent electrical conductivity and chemical stability, and are widely used in fuel cells and chlor-alkali batteries, but there are still many shortcomings, such as the electrical conductivity is not high enough, and the normal temperature of its single film Conductivity (Conductivity) <0.1 (S / cm); high chemical penetration, unable to effectively block the penetration of toxic and harmful chemicals
[0003] Expanded polytetrafluoroethylene is prepared by using high-crystallinity polytetrafluoroethylene dispersion resin, which is obtained by biaxial stretching and expansion. It has a microporous structure closely combined with micron or nanofibers, and has excellent physical and chemical properties and mechanical properties. Waterproof, breathable and chemically stable, it has been used to manufacture wire and cable insulation materials, artificial blood vessels, sealing tapes, environmental protection filters, and clothing fabrics since the 1970s; but its disadvantage is that these micron or nanofibers are not puncture resistant. Well, the creep resistance is not good, and these micron or nanofibers will continue to be stretched and loosened after tension, resulting in deformation of the membrane structure, resulting in a decline in functionality, which seriously affects the overall protective function of the membrane

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] A preparation method of fluorine-containing chlorine-containing conductive polymer resin, comprising the steps of:

[0023] S1 Add 1% to 20% of free-radical polymerizable fluorine-containing liquid phase monomer with sulfonyl fluoride, 79% to 98% of purified water, and 0.01% to 1% of fluorine-containing surfactant into the reactor by weight percentage for high-speed Stir to obtain prepolymer emulsion;

[0024] S2 Into the reaction kettle, one or both of tetrafluoroethylene and vinylidene fluoride and the gas phase mixed monomer of chlorotrifluoroethylene are introduced, and the reaction pressure is 5 kg or more; then a free radical initiator is introduced, and the reaction temperature is At 20-120°C, the reaction pressure is 5-25 kg, and the reaction time is 15-180 minutes, and the reaction product is a polymer emulsion containing fluorine and chlorine with sulfonyl fluoride; the liquid phase monomer containing fluorine and sulfonyl fluoride is combined with The ratio ...

Embodiment 1

[0036] In a closed pre-emulsification reaction kettle A with an internal volume of about 100 liters, add 39000g of pure water and 100g of perfluorooctanoic acid ammonium at room temperature, turn on high-speed shear stirring, and then slowly add 5000g of 70% CF by weight into the kettle 2 = CF-O-CF 2 CFCF 3 -O-CF 2 CF 2 -SO 2 F and 30% CF 2 = CF-O-CF 2 CF 2 -SO 2 F mixed liquid-phase monomers containing fluorine and sulfonyl fluoride, after continuous high-speed shearing and stirring for about 30 minutes, a prepolymer emulsion was prepared;

[0037] In another reaction kettle B with an internal volume of about 100 liters, the oxygen in the kettle is exhausted until the oxygen content in the kettle is less than 20ppm, and then all the prepolymer emulsion from the reactor A is added, and the gas phase mixed monomer is introduced into the kettle , the molar ratio of which is 90% tetrafluoroethylene and 10% chlorotrifluoroethylene, the temperature is raised to 70 degrees, ...

Embodiment 2

[0041] In a closed pre-emulsification reaction kettle A with an internal volume of about 100 liters, add 39000g deionized water and 100g ammonium perfluorooctanoate at room temperature, turn on high-speed shear stirring, and then slowly add 5000g of 80% CF by weight into the kettle 2 = CF-O-CF 2 CFCF 3 -O-CF 2 CF 2 -SO 2 F and 20% CF 2 = CF-O-CF 2 CF 2 -SO 2 The mixture of F, after continuous high-speed shearing and stirring for about 30 minutes, a prepolymer emulsion was obtained; in another reactor B with an internal volume of about 100 liters, oxygen was first exhausted in the reactor until the oxygen content in the reactor was less than 20ppm, and then Add all the prepolymer emulsion from the reactor A, and feed the mixed gas-phase mixed monomer into the kettle, the molar ratio of which is 75% tetrafluoroethylene, 20% vinylidene fluoride and 5% chlorotrifluoroethylene, and heat up to 70 degrees , the pressure in the kettle was maintained at 9 kg, and 2.5 g of ammon...

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Abstract

The invention discloses a fluorine and chlorine-containing conducting polymer resin preparation method. The fluorine and chlorine-containing conducting polymer resin preparation method comprises the following steps of: firstly mixing and blending a fluorine-containing liquid phase monomer with sulfuryl fluoride and polymerizable free radicals, purified water and a fluorine-containing surfactant to obtain prepolymer emulsion; then feeding a vapor-phase mixed monomer and a free radical initiator to carry out radical polymerization to obtain fluorine and chlorine-containing polymer emulsion with sulfuryl fluoride; and finally hydrolyzing the fluorine and chlorine-containing polymer emulsion with sulfuryl fluoride, condensing, washing and drying to obtain fluorine and chlorine-containing conducting polymer resin. The fluorine and chlorine-containing conducting polymer resin obtained by the preparation method has excellent physical and chemical properties such as relatively mechanical strength, water resistance, water vapor permeability, oil resistance, washing resistance, flame resistance, biochemical weapon penetration resistance and high conductivity.

Description

technical field [0001] The invention relates to the technical field of molecular materials, in particular to a preparation method of a fluorine- and chlorine-containing conductive polymer resin. Background technique [0002] Fluorine-containing polymers, especially homopolymerized, modified, or copolymerized polymer resins of tetrafluoroethylene have excellent physical and mechanical properties and chemical stability, and are used in chemical materials, mechanical electronics, aerospace, military protection, new materials and New energy and other fields have a wide range of applications; chlorine-containing polymers, such as homopolymerized, modified, or copolymerized polymer resins of chlorotrifluoroethylene, have excellent physical and mechanical properties and resistance to chemical penetration. made important contributions. Fluorine-containing conductive polymers such as DuPont's Nafion resin have excellent electrical conductivity and chemical stability, and are widely ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F261/06C08F214/26C08F214/22C08F214/24
CPCC08F261/06C08F214/262C08F214/222C08F214/242
Inventor 吴慧生杨颖
Owner ZHEJIANG HYPROOF TECH CO LTD
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