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Perfluorinated ion exchange membrane with evenly-distributed cross-linking points and preparing method and application thereof

A technology with uniform distribution and perfluorinated ions, used in fuel cells, electrochemical generators, electrical components, etc., can solve the problems of uneven distribution of cross-linking points, decreased mechanical strength, and decreased exchange capacity, and achieves the distribution of cross-linking points. Effects of uniformity, improved mechanical properties, high exchange capacity and electrical conductivity

Active Publication Date: 2017-02-22
SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to provide a perfluorinated ion-exchange membrane with uniform distribution of cross-linking points, which solves the problems of uneven distribution of cross-linking points and decreased exchange capacity in the existing sulfonimide cross-linked perfluorinated ion-exchange membranes And the problem that the mechanical strength decreases when increasing the ion exchange capacity of the perfluorosulfonic acid resin has the characteristics of uniform distribution of crosslinking points and high exchange capacity. The present invention also provides its preparation method and application

Method used

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  • Perfluorinated ion exchange membrane with evenly-distributed cross-linking points and preparing method and application thereof
  • Perfluorinated ion exchange membrane with evenly-distributed cross-linking points and preparing method and application thereof
  • Perfluorinated ion exchange membrane with evenly-distributed cross-linking points and preparing method and application thereof

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Embodiment 1

[0046] The preparation process of perfluorosulfonamide resin is as follows:

[0047] The reactor was washed, wiped dry, and purged with nitrogen, then 200g of perfluorosulfonyl fluoride resin flake pellets with sulfonyl fluoride side chains were placed in a 2L stainless steel autoclave, 700mL DMF was added, and vacuum was applied to 0.1mbar, the temperature of the kettle body low-temperature circulating cooling pump is cooled to -20±2℃, and 40g NH is added to the reaction kettle through the gas feed valve 3 , Slowly warm up to 0±2℃, stir the reaction for 70h, stop stirring; through the gas feed valve, inject 0.4kPa compressed air into the reactor, then close the gas feed valve, open the liquid discharge valve, and use pressure to remove the solvent And the remaining ammonia gas is injected into the solvent recovery bottle, and water is used to absorb the remaining ammonia gas from the reaction; the resin particles in the reactor are cleaned and dried in an oven at 120°C to obtain ...

Embodiment 2

[0050] The preparation process of perfluorosulfonamide resin is as follows:

[0051] The reactor was washed, wiped dry, and purged with nitrogen. Then 200g of perfluorosulfonyl fluoride resin flake pellets with sulfonyl fluoride side chains were placed in a 2L stainless steel autoclave, 500mL of anhydrous acetonitrile was added, and pumped Vacuum to 0.1mbar, cool down to -20±2℃ by the low-temperature circulation cooling pump of the kettle body, add 40g NH3 into the reactor through the gas feed valve, slowly raise the temperature to 25±2℃, stir and react for 24h, stop stirring; The feed valve, press 0.4kPa compressed air into the reactor, then close the gas feed valve, open the liquid discharge valve, use pressure to pump the solvent and remaining ammonia into the solvent recovery bottle, and use water to absorb the remaining ammonia from the reaction ; Clean the resin particles in the reactor and dry them in an oven at 120°C to obtain the perfluorosulfonamide resin. The target pr...

Embodiment 3

[0053] The preparation process of perfluorosulfonamide resin is as follows:

[0054] The reactor was washed, wiped dry, and purged with nitrogen, then 200g of perfluorosulfonyl fluoride resin flake pellets with sulfonyl fluoride side chains were placed in a 2L stainless steel autoclave, and 500mL anhydrous 1,4 -Dioxane, vacuum to 0.1mbar, cool down to -20±2℃ by the low-temperature circulating cooling pump of the kettle body, add 20g NH to the reaction kettle through the gas feed valve 3 , Slowly warm up to 25±2℃, stir the reaction for 24h, stop stirring; through the gas feed valve, inject 0.4kPa compressed air into the reactor, then close the gas feed valve, open the liquid discharge valve, and use pressure to remove the solvent And the remaining ammonia gas is injected into the solvent recovery bottle, and water is used to absorb the remaining ammonia gas; the resin particles in the reactor are cleaned and dried in an oven at 120°C to obtain the perfluorosulfonamide resin. The ta...

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Abstract

The invention relates to a perfluorinated ion exchange membrane with evenly-distributed cross-linking points and a preparing method and application thereof, and belongs to the technical field of fluorine-containing high polymer materials. The preparing method includes the steps that a tetrafluoroethylene monomer and a perfluorinated sulfonyl halide vinyl ether monomer are copolymerized to generate perfluorinated sulfonyl halide resin, then the perfluorinated sulfonyl halide resin and ammonia are subjected to an ammonolysis reaction, and the perfluorinated sulfamide resin is obtained; the perfluorinated sulfamide resin serves as a cross-linking agent, the perfluorinated sulfonyl halide resin serves as matrix resin, the perfluorinated sulfamide resin and the perfluorinated sulfonyl halide resin are melted and blended to be extruded and subjected to membrane forming, or are prepared into a solution to be subjected to curtain coating and membrane forming respectively, then the product is soaked into an organic solvent, subjected to a cross-linking reaction under the catalytic effect of organic alkali, hydrolyzed, acidized and washed, and then the perfluorinated ion exchange membrane with the evenly-distributed cross-linking points is obtained. The exchange membrane has the chemical stability, also has the high exchange capacity and the high conductivity, and particularly, has the high mechanical strength and the dimensional stability, and the perfluorinated ion exchange membrane is suitable for field applications such as fuel cells, vanadium cells, electrolysis water and electrolysis experiment / gas dehumidification.

Description

Technical field [0001] The invention relates to a perfluorinated ion exchange membrane with uniform distribution of crosslinking points, a preparation method and application thereof, and belongs to the technical field of fluorine-containing polymer materials. Background technique [0002] The perfluorinated ion exchange membrane is a perfluorosulfonic acid proton exchange membrane (Nafion) first developed by DuPont in the United States in 1962. It is a copolymer of tetrafluoroethylene and perfluorosulfonic acid vinyl ether. Compared with non-fluorine hydrocarbon ion exchange membranes, perfluorosulfonic acid ion exchange membranes have the advantages of excellent chemical and electrochemical stability and long life. They have been successfully commercialized and are used in ion-exchange membrane electrolyzers in the chlor-alkali industry. Proton exchange membrane fuel cells (Proton exchange membrane fuelcells, abbreviated as PEMFCs). [0003] The proton exchange membrane fuel cell...

Claims

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Application Information

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IPC IPC(8): C08J5/22C08J3/24C08L27/18H01M8/1072H01M8/1081H01M8/1039
CPCC08J3/246C08J5/2237C08J2327/18C08J2427/18H01M8/1039H01M8/1072H01M8/1081Y02E60/50
Inventor 高红荣张永明董辰生
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD