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Densely sulfonated polyaryletherketone/SiO2 composite proton exchange membrane and preparation method thereof

A sulfonated polyaryl ether ketone and proton exchange membrane technology, which is applied in electrochemical generators, fuel cells, electrical components, etc. The effect of low vanadium ion permeability, easy availability, and high ion selectivity

Active Publication Date: 2020-08-14
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the high surface energy of inorganic nanofillers, it is easy to agglomerate together in the process of film formation, and it is difficult to distribute uniformly in the polymer matrix, making it difficult to achieve the expected performance of the composite film. The exchange membrane solution tends to settle after a long period of time, which brings difficulties to the actual preparation

Method used

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  • Densely sulfonated polyaryletherketone/SiO2 composite proton exchange membrane and preparation method thereof
  • Densely sulfonated polyaryletherketone/SiO2 composite proton exchange membrane and preparation method thereof
  • Densely sulfonated polyaryletherketone/SiO2 composite proton exchange membrane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Embodiment 1 The preparation of polyaryletherketone compound PAE-8%

[0048] The polymerization reaction uses a three-necked flask with a condenser, a water separator, and is equipped with argon gas protection inlet and outlet, and corresponding magnetic stirring devices. Add 0.3300g (0.32mmol) bisphenol monomer containing dense electron-rich benzene rings, 0.9201g (3.68mmol) 4,4'-dihydroxydiphenyl sulfone, 0.8728g (4.00mmol) to a 25mL round bottom three-neck flask, 0.8728g (4.00mmol) , 4'-difluorobenzophenone, 0.8298 g (6 mmol) anhydrous potassium carbonate, 10.5 mL N,N-dimethylacetamide and 5 mL toluene. Under the protection of nitrogen atmosphere, raise the temperature to 145-150°C, reflux for 2 hours to remove the water molecules produced by the reaction, then discharge the toluene in the water separator, continue the reaction for 1 hour to remove the toluene in the reaction solution, and then raise the temperature to 165°C to continue the reaction 20h. After the ...

Embodiment 2

[0050] Example 2 Preparation of dense sulfonated polyaryletherketone compound SPAE-8%

[0051] In a 1000mL three-necked round-bottomed flask equipped with a constant pressure titration funnel, an argon-protected inlet and outlet, and a magnetic stirring device, add 1.01g (2.04mmol) of the polyaryletherketone compound PAE-8% obtained in Example 1, and then add 400 mL of dichloromethane. After the polymer is completely dissolved, quickly take 1.07mL of chlorosulfonic acid and dissolve it in a constant pressure titration funnel filled with 20mL of dichloromethane, and drop it into a three-necked flask at a rate of 0.5 drops / second, and obtain an adhesion after 24 hours of reaction. The brown precipitate on the glass wall, the precipitate was washed three times with dichloromethane, dissolved with 30mL DMAc, neutralized with 0.4M sodium hydroxide solution to a pH value of 7, poured into a dialysis bag, and dialyzed in deionized water for three days, changing every day water three...

Embodiment 3

[0052] Example 3 dense sulfonated polyaryletherketone / SiO 2 Composite Proton Exchange Membrane SPAE / SiO 2 Preparation of -4

[0053] Take 1g of the dense sulfonated polyaryletherketone compound SPAE-8% obtained in Example 2, dissolve it completely in 20mL of N,N-dimethylacetamide, add 0.149mL of ethyl orthosilicate dropwise with a pipette gun, and Shake for 1 hour, then expose to the air and continue magnetic stirring for 24 hours, finally cast on a horizontal glass plate, dry at 80°C for 12 hours, then continue to dry at 80°C for 12 hours in vacuum, then soak in deionized water to peel off SPAE / SiO produced by film production 2 -4 Composite film.

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Abstract

The invention belongs to the field of proton exchange membrane materials, and particularly relates to a densely sulfonated polyaryletherketone / SiO2 composite proton exchange membrane and a preparationmethod thereof. The preparation method comprises the following steps: preparing a polyaryletherketone compound from a bisphenol monomer containing dense electron-rich benzene rings, 4,4'-dihydroxy diphenyl sulfone and 4,4'-difluorobenzophenone through a high-temperature polycondensation reaction; selectively sulfonating electron-rich benzene ring chain segments with chlorosulfonic acid to obtaina densely sulfonated polyaryletherketone compound; and by taking the densely sulfonated polyaryletherketone as a matrix, introducing SiO2 through sol-gel reaction of tetraethoxysilane, and performingsolution casting to form a membrane, thereby obtaining the densely sulfonated polyaryletherketone / SiO2 composite proton exchange membrane. The composite proton exchange membrane prepared by the methodhas the advantages of high proton conductivity, good SiO2 dispersion, excellent dimensional stability and mechanical properties, low vanadium ion permeability, high ion selectivity and the like, andhas a good application prospect in the field of all-vanadium redox flow battery diaphragms.

Description

technical field [0001] The present invention relates to a dense sulfonated polyaryletherketone / SiO 2 A composite proton exchange membrane belongs to the field of proton exchange membrane materials. Background technique [0002] Unlike traditional batteries, the energy of a vanadium redox flow battery (VRB) is stored in the active material of the electrolyte, and the inert electrode itself has no electrochemical reaction, so the energy storage and power output of VRB are relatively independent. In the case of a certain number of stacks, the battery capacity can be achieved by increasing the volume or concentration of the electrolyte. In addition to the flexibility of system design and safety and environmental protection, VRB is very suitable for the requirements of large-scale electrochemical energy storage. It has developed rapidly in recent years. The application prospect is more and more broad. [0003] Proton exchange membrane (PEM) is an important type of VRB separator...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/22C08L81/06C08K3/36C08G75/23H01M8/1051H01M8/1072H01M8/18
CPCC08G75/23C08J5/2256C08J2381/06C08K3/36H01M8/1051H01M8/1074H01M8/188Y02E60/50
Inventor 陈栋阳郑子桂陈男杰
Owner FUZHOU UNIV
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