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A kind of sulfonated polyphenylene ether ketone and preparation method thereof, sulfonated polyphenylene ether ketone proton exchange membrane

A technology of sulfonated polyphenylene ether ketone and proton exchange membrane, which is applied in the field of polymers, can solve problems such as poor interface compatibility, battery performance degradation, deformation or shedding, and achieve low methanol permeability, low cost, and high proton conductivity rate effect

Active Publication Date: 2016-06-01
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the interfacial compatibility between the sulfonated polyphenylene proton exchange membrane material and the catalytic layer is poor, and defects such as cracking, deformation or shedding occur during the processing of the membrane electrode (MEA), which makes the battery performance decline significantly.

Method used

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  • A kind of sulfonated polyphenylene ether ketone and preparation method thereof, sulfonated polyphenylene ether ketone proton exchange membrane
  • A kind of sulfonated polyphenylene ether ketone and preparation method thereof, sulfonated polyphenylene ether ketone proton exchange membrane
  • A kind of sulfonated polyphenylene ether ketone and preparation method thereof, sulfonated polyphenylene ether ketone proton exchange membrane

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preparation example Construction

[0061] The present invention provides the preparation method of sulfonated poly(phenylene ether ketone) described in the technical scheme, comprising the following steps:

[0062] Under the action of a catalyst, the monomer having the structure shown in formula VII is polymerized with the sulfonated monomer in an organic solvent to obtain the sulfonated poly(phenylene ether ketone) having the structure shown in formula I;

[0063] RO-Ar-OR formula VII;

[0064] In formula VII, Ar is selected from any one of the structures shown in formula II to formula VI:

[0065]

[0066] R is

[0067] The sulfonated monomer has a structure shown in formula VIII:

[0068]

[0069] In the present invention, under the action of a catalyst, the monomer having the structure shown in formula VII is polymerized with the sulfonated monomer having the structure shown in formula VIII in an organic solvent to obtain the sulfonated monomer having the structure shown in formula I. Polyphenyle...

Embodiment 1

[0186] Add 4.65g of 4-chloro-4'-hydroxybenzophenone (20mmol), 1.39g of 2,6-difluorobenzonitrile (10mmol) and 3.04g of potassium carbonate (22mmol) into 30mL of DMAc, and under nitrogen protection, the obtained The mixed solution was heated to 80° C. for 6 h; after cooling to room temperature, the reaction solution was poured into 200 mL of water, and a white solid was precipitated, which was filtered and dried to obtain the target compound.

[0187] The present invention carries out the proton nuclear magnetic resonance spectrum detection with the target compound that obtains, and the result is: 1 HNMR (300MHz, DMSO; ppm): δ7.87(d, 4H, J=9.0Hz), 7.78(d, 4H, J=9.0Hz), 7.71(d, 1H, J=9.0Hz), 7.65(d ,4H,J=9.0Hz),7.37(d,4H,J=9.0Hz),7.01(d,2H,J=9.0Hz). 13 CNMR (75MHz, DMSO; ppm): δ194.1, 159.8, 158.4, 139.0, 135.7, 134.6, 133.6, 132.3, 131.3, 128.8, 118.9, 112.6, 112.1, 97.5.

[0188] The target compound obtained by the present invention is subjected to mass spectrometry, and the ...

Embodiment 2

[0193] 4.69 g of 4-chloro-4'-fluorobenzophenone (20 mmol), 1.10 g of resorcinol (10 mmol) and 3.04 g of potassium carbonate (22 mmol) were added to 30 mL of DMAc. Under the protection of nitrogen, the obtained mixed solution was heated to 80° C. for 12 h; after cooling to room temperature, the reaction solution was poured into 200 mL of water, and a white solid was precipitated, which was filtered and dried to obtain the target compound.

[0194] The present invention carries out proton nuclear magnetic resonance spectrum analysis with the target compound that obtains, and the result is: 1 HNMR (300MHz, DMSO; ppm): δ7.80(d, 4H, J=9.0Hz), 7.74(d, 4H, J=9.0Hz), 7.62(d, 4H, J=9.0Hz), 7.54(t ,1H,J=9.0Hz),7.18(d,4H,J=9.0Hz),7.02(dd,2H,J=9.0Hz,J=3.0Hz),6.96(d,1H,J=3.0Hz).

[0195] The present invention carries out mass spectrometry to the target compound that obtains, and the result is: ESMS:539.2 (M+H) + ;

[0196] As can be seen from the analysis results of the above-menti...

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Abstract

The invention provides a sulfonated polyphenylether ketone disclosed as Formula I and a proton exchange membrane prepared by using the sulfonated polyphenylether ketone as a film-forming polymer. The monomer proportion (m / n) can be regulated to well regulate the glass transition temperature of the obtained sulfonated polyphenylether ketone so as to obtain the sulfonated polyphenylether ketone with lower glass transition temperature, thereby solving the problem of hot press generated by higher glass transition temperature of the polyphenyl proton exchange membrane. The proton exchange membrane prepared from the sulfonated polyphenylether ketone has the advantages of low methanol permeability, favorable oxidation stability and higher proton conductivity. The experimental result indicates that the methanol permeability of the proton exchange membrane can be down to 0.23*10<-6>cm<2>S<-1>, the oxidation stability is 99 wt% or so, and the glass transition temperature is 190 DEG C or so.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to a sulfonated poly(phenylene ether ketone), a preparation method thereof and a proton exchange membrane. Background technique [0002] The source of methanol is abundant, and it is easy to carry and store. Direct methanol fuel cells (DMFC) can achieve zero or low emissions and other advantages, which have attracted widespread attention. Proton exchange membrane is the core component of DMFC. It plays the role of blocking fuel and oxidant, and conducting protons. It is a polymer separation membrane that is selectively permeable. Its performance largely determines the performance of fuel cells. [0003] At present, the proton exchange membrane widely used in DMFC is the fluorine-containing sulfonic acid type proton exchange membrane, such as series membrane (DuPont), Series membrane (AsahiChemical company), Membrane (AsahiGlass), Membrane (Dow Corporation). Although this t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G61/12C08J5/22H01M4/86H01M8/02H01M8/0297
CPCY02E60/50
Inventor 郑吉富何庆一毕伟辉代磊张所波
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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