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Doped and crosslinked multilayer perfluorinated ionic membrane and preparation method thereof

A perfluorinated ion and ion membrane technology, applied in the field of functional polymer composite materials, can solve the problems of reduced membrane strength, poor dimensional stability, and reduced equivalent value, and achieve improved high-temperature electrical conductivity, improved mechanical properties, and tight bonding. Effect

Active Publication Date: 2010-08-11
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

[0003] Although the current perfluorosulfonic acid proton exchange membrane has been used for many years, there are still many defects that cannot meet the requirements of commercialization: low proton conductivity at high temperature, poor dimensional stability, low mechanical strength, etc.
[0005] US20070031715 describes the cross-linking method of sulfonyl chloride cross-linking to generate sulfonyl anhydride, but the cross-linking structure has obvious disadvantages: the sulfonyl anhydride unit is unstable to alkali
Generally speaking, when the ion exchange capacity increases, the equivalent value of the perfluoropolymer decreases (the equivalent value EW value decreases, the ion exchange capacity IEC=1000 / EW), and the strength of the membrane also decreases, and the membrane strength The gas permeability also increases, which will have a very serious impact on the fuel cell

Method used

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  • Doped and crosslinked multilayer perfluorinated ionic membrane and preparation method thereof
  • Doped and crosslinked multilayer perfluorinated ionic membrane and preparation method thereof
  • Doped and crosslinked multilayer perfluorinated ionic membrane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Convert the repeating unit to

[0074]

[0075] , polymer resin with EW=1000 and Zr(HPO 4 ) 2 (Zr(HPO 4 ) 2 The mass ratio of resin to resin is 3:100) mixed in propanol-water to obtain a solution, and then MnCO was added to the above solution 3 (accounting for 0.01% of the resin mass), make a total mass concentration of 5% propanol-water solution, then add it to the 5% perfluoromalonyl peroxide DMF solution, fully disperse and cast it to a horizontal position In the polytetrafluoroethylene casting mold, after vacuum drying at 80°C for 12 hours, the film was peeled off, and the molar concentration of 0.5M H 2 SO 4 The solution was boiled for 1 hour and washed with deionized water. After the heat treatment, the membrane was sequentially treated with NaOH solution and sulfuric acid solution to obtain a doped ion membrane (single-layer membrane 1#) with a cross-linking bridge (I). The above two single-layer perfluorinated cross-linked ion-doped membranes were stac...

Embodiment 2

[0077] Convert the repeating unit to

[0078]

[0079] , polymer resin with EW=700, SiO with a particle size of 0.03 μm 2 (SiO 2 The mass ratio of perfluorosulfonic acid resin is 5:100) and Ce with perovskite structure x Ti (1-x) o 2 (x=0.4) The oxide (accounting for 2% of the mass of the resin) was fully extruded at 200° C. to obtain a film with a thickness of 30 μm. Soak the membrane in NH 4 Cl in DMF for 5 hours. The soaked membrane was then placed in triethylamine at 200 °C for 2 hours to obtain a crosslinked membrane. The membrane was sequentially treated with KOH solution and hydrochloric acid solution to obtain an ion exchange membrane (single-layer membrane 2#) with a cross-link bridge (II).

[0080] Place the above ionic membrane in the repeating unit as

[0081]

[0082] EW = 1200 polymer resin and tetraphenyl tin mixture, and at 270 ° C with a twin-screw extruder to obtain a film thickness of 50 μm, and then add the film at 230 ° C for 10 hours to obta...

Embodiment 3

[0084] Convert the repeating unit to

[0085]

[0086] , EW=1100 polymer resin and La 0.7 Ce 0.15 Ca 0.15 MnO 3 (accounting for 1% of the resin mass) and urea by hot pressing to obtain a film with a thickness of 100 μm. After heating the film at 170 ° C for 5 hours, it was treated with alkali and acid in sequence to obtain ions with cross-linking bridges (II) Membrane (single layer membrane 4#).

[0087] Convert the repeating unit to

[0088]

[0089] , polymer resin of EW=940, La-DMSO complex (accounting for 0.007% of resin mass) and H 3 PW 12 o 40 , by polymer resin with H3 PW 12 o 40 The ratio of the mass ratio of 100:20 was made into a DMSO solution with a mass concentration of 30%, and a film (monolayer film 5#) with a thickness of 10 μm was obtained by casting at 170° C. for 60 minutes.

[0090] The single-layer membranes 4# and 5# are stacked for hot pressing, and then hot-pressed with the multilayer membrane 2# to obtain a six-layer cross-linked doped i...

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Abstract

The invention relates to a doped and crosslinked multilayer perfluorinated ionic membrane and a preparation method thereof, and belongs to the field of functional polymer composite materials. The fluoride-containing ion exchange membrane has a multilayer structure. The fluoride-containing ion exchange resin serves as a membrane-forming resin; proton conduction assisting materials and highvalent metallic compounds are added therein at the same time to perform a crosslinking reaction under a certain condition so as to form the doped ion exchange membrane having a network structure. The ion exchange membrane prepared by the method of the invention has the advantages of higher proton conductivity, size stability, and chemical stability, particularly extremely excellent gas-permeation resistant performance.

Description

technical field [0001] The invention belongs to the field of functional polymer composite materials, and relates to a fluorine-containing ion exchange membrane and a preparation method thereof. Background technique [0002] Proton exchange membrane fuel cell is a power generation device that directly converts chemical energy into electrical energy by electrochemical means, and is considered to be the preferred clean and efficient power generation technology in the 21st century. Proton exchange membrane (proton exchange membrane, PEM) is the key material of proton exchange membrane fuel cell (proton exchange membrane fuel cell, PEMFC). [0003] Although the current perfluorosulfonic acid proton exchange membrane has been used for many years, there are still many defects that cannot meet the requirements of commercialization: low proton conductivity at high temperature, poor dimensional stability, and low mechanical strength. Especially in terms of dimensional stability, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/32H01M8/02H01M2/16C08L27/18C08K3/28C08K3/30C08K3/26C08K3/32C08K5/098C08L5/16C08K3/22C08K3/34C08K3/36C08J3/24C08J5/22H01M8/1039
CPCY02E60/12Y02E60/50
Inventor 张永明唐军柯刘萍张恒王军
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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