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Epoxy resin semi-interpenetrating network sulfonated poly[(5-p-aminobenzene sulfonic acid)cyclotriphosphazene-ether ether ketone] proton exchange membrane material and preparation method thereof

A technology for sulfonating polyether ether ketone and p-aminobenzenesulfonic acid, which is used in epoxy resin semi-interpenetrating network sulfonated poly[(penta-p-aminobenzenesulfonic acid) cyclotriphosphazene-ether ether ketone] proton exchange In the field of membrane materials and their preparation, it can solve the problems of high alcohol permeability coefficient and water swelling rate, high proton conductivity, low proton conductivity, etc., and achieve the effect of reducing swelling effect, low preparation cost, and high electrical conductivity

Inactive Publication Date: 2015-03-25
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the SPEEK membrane with high sulfonation degree (DS>90%) has higher proton conductivity, alcohol permeability coefficient and water swelling rate are higher, and even fails due to excessive swelling; while low sulfonation degree (DS<40% ) SPEEK membrane has excellent alcohol resistance and water swelling resistance, but the proton conductivity is low, far inferior to Nafion membrane

Method used

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  • Epoxy resin semi-interpenetrating network sulfonated poly[(5-p-aminobenzene sulfonic acid)cyclotriphosphazene-ether ether ketone] proton exchange membrane material and preparation method thereof
  • Epoxy resin semi-interpenetrating network sulfonated poly[(5-p-aminobenzene sulfonic acid)cyclotriphosphazene-ether ether ketone] proton exchange membrane material and preparation method thereof
  • Epoxy resin semi-interpenetrating network sulfonated poly[(5-p-aminobenzene sulfonic acid)cyclotriphosphazene-ether ether ketone] proton exchange membrane material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Dissolve (1.7000g, 0.0050mol) SPEEK (65% sulfonation degree) in 30 mL of DMAc solvent in a 100 mL three-neck flask equipped with magnetic rotor stirring, condenser, and thermometer, and turn on the magnetic force Stir, and heat the oil bath to 60°C to prepare a film-forming solution;

[0035] (2) Under nitrogen protection, add (0.1892g, 0.0050mol) NaBH at one time to the film-forming solution obtained in step (1) 4 , heated to 100°C for reflux reaction for 12 hours, centrifuged and purified to obtain the supernatant;

[0036] (3) Dissolve (0.1738g, 0.0005mol) hexachlorocyclotriphosphazene in DMAc solvent in a 500mL three-necked flask equipped with magnetic rotor stirring, condenser, and HCl absorption device, and add step (2) dropwise The resulting supernatant was stirred and reacted in an ice-water bath for 24 hours.

[0037] (4) In a 500mL three-neck flask equipped with magnetic rotor stirring, condenser, and HCl absorption device, under nitrogen protection, add...

Embodiment 2

[0063] (1) Dissolve (3.4000g, 0.0100mol) SPEEK (69% sulfonation degree) in 30 mL of DMAc solvent in a 100 mL three-necked flask equipped with magnetic rotor stirring, condenser, and thermometer, and turn on the magnetic force Stir and heat the oil bath to 100°C to prepare a film-forming solution;

[0064] (2) Under the protection of nitrogen, add (0.3783g, 0.0100mol) NaBH4 to the membrane-forming solution obtained in step (1) at one time, raise the temperature to 90°C for reflux reaction for 18 hours, centrifuge and purify, and obtain the supernatant;

[0065] (3) Dissolve (0.3477g, 0.0010mol) hexachlorocyclotriphosphazene in DMAc solvent in a 500mL three-neck flask equipped with magnetic rotor stirring, condenser, and HCl absorption device, and add step (2) dropwise The resulting supernatant was stirred and reacted in an ice-water bath for 24 hours.

[0066] (4) In a 500mL three-neck flask equipped with magnetic rotor stirring, condenser, and HCl absorption device, under the...

Embodiment 3

[0077] (1) Dissolve (2.0400g, 0.0060mol) SPEEK (sulfonation degree 75) in 30 mL of DMAc solvent in a 100 mL three-necked flask equipped with magnetic rotor stirring, condenser, and thermometer, and turn on the magnetic stirring , heat the oil bath to 100°C, and prepare a film-forming solution;

[0078] (2) Under the protection of nitrogen, add (0.2270g, 0.0060mol) NaBH4 to the membrane-forming solution obtained in step (1) at one time, heat up to 120°C for reflux reaction for 10 hours, centrifuge and purify, and obtain the supernatant;

[0079] (3) Dissolve (0.3129g, 0.0009mol) hexachlorocyclotriphosphazene in DMAc solvent in a 500mL three-neck flask equipped with magnetic rotor stirring, condenser, and HCl absorption device, and add step (2) dropwise The resulting supernatant was stirred and reacted in an ice-water bath for 24 hours.

[0080] (4) In a 500mL three-necked flask equipped with a magnetic rotor stirring, a condenser, and an HCl absorption device, under nitrogen p...

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Abstract

The invention relates to an epoxy resin semi-interpenetrating network sulfonated poly[(5-p-aminobenzene sulfonic acid)cyclotriphosphazene-ether ether ketone] proton exchange membrane material and a preparation method thereof. The proton exchange membrane material is formed by making cyclotriphosphazene derivative grafted-modified sulfonated poly(ether ether ketone) which serves as a linear chain penetrate through the crosslinked network which serves as a main body and is formed by epoxy resin, wherein the mass ratio of the cyclotriphosphazene derivative grafted-modified sulfonated poly(ether ether ketone) to the crosslinked network formed by epoxy resin is 1:(0.2-1.5). The proton exchange membrane material prepared by adopting the method has the characteristics of low production cost, high conductivity, good alcohol hindering performance and good heat resistance. The conductivity at a temperature of 20-90 DEG C of the proton exchange membrane material is 1.80*10<-3>-5.10*10<-1>S.cm<-1>, the alcohol hindering coefficient is 2.00*10<-7>-9.0*10<-7>cm<2>.s<-1> and the water absorption is 12-100%.

Description

technical field [0001] The invention relates to an epoxy resin semi-interpenetrating network sulfonated poly[(penta-p-aminobenzenesulfonic acid)cyclotriphosphazene-ether ether ketone] proton exchange membrane material and a preparation method thereof. Background technique [0002] Direct methanol fuel cell (DMFC) has attracted much attention in recent years for its advantages of high efficiency, high energy density, low emission and using renewable methanol as fuel. As the core component of DMFC, proton exchange membrane (PEM) plays a dual role of isolating fuel and conducting protons. Its performance is closely related to the life and performance of DMFC. [0003] At present, the more successful PEM is the perfluorosulfonic acid membrane represented by Dupont's Nafion membrane. This membrane has good chemical stability and high electrical conductivity, but it also has some defects, such as high cost, The performance degradation at high temperature (above 100°C) and poor al...

Claims

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Application Information

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IPC IPC(8): C08L61/16C08L63/00C08J5/22C08G8/28
Inventor 郭强张天骄毕宸洋余舟张豪东尹泽辉
Owner SHANGHAI UNIV
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