Sulfonated poly[(penta-sulfanilic acid)phosphonitrilic-polyetherether ketone] proton exchange membrane material and preparation method thereof

A technology of p-aminobenzenesulfonic acid and sulfonated polyether ether ketone, which is applied to fuel cell parts and components, can solve the problems of high alcohol penetration coefficient and water swelling rate, low proton conductivity, and high proton conductivity, and achieve Effects of reduced swelling, low production cost, and high electrical conductivity

Inactive Publication Date: 2015-01-07
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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  • Sulfonated poly[(penta-sulfanilic acid)phosphonitrilic-polyetherether ketone] proton exchange membrane material and preparation method thereof
  • Sulfonated poly[(penta-sulfanilic acid)phosphonitrilic-polyetherether ketone] proton exchange membrane material and preparation method thereof
  • Sulfonated poly[(penta-sulfanilic acid)phosphonitrilic-polyetherether ketone] proton exchange membrane material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Dissolve (1.7000g, 0.0050mol) SPEEK (sulfonation degree 65) 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 stirring , heat the oil bath to 50°C, and make a film-making solution;

[0028] (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;

[0029] (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.

[0030] (4) In a 500mL three-neck flask equipped with magnetic rotor stirring, condenser, and HCl absorption device, under nitrogen protection, add (0.4330...

Embodiment 2

[0055] (1) Dissolve (3.4000g, 0.0100mol) SPEEK (sulfonation degree 65) 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 stirring , heat the oil bath to 50°C, and make a film-making solution;

[0056] (2) Under the protection of nitrogen, add (0.3783g, 0.0100mol) NaBH4 to the film-forming solution obtained in step (1) at one time, heat up to 80°C for reflux reaction for 20 hours, centrifuge and purify, and obtain the supernatant;

[0057] (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.

[0058] (4) In a 500mL three-neck flask equipped with magnetic rotor stirring, condenser, and HCl absorption device, under the protection of nitrogen, add...

Embodiment 3

[0068] (1) Dissolve (2.0400g, 0.0060mol) SPEEK (sulfonation degree 65) 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 50°C, and make a film-making solution;

[0069] (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;

[0070] (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.

[0071] (4) In a 500mL three-necked flask equipped with a magnetic rotor stirring, a condenser, and an HCl absorption device, under nitrogen protec...

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Abstract

The invention relates to a sulfonated poly[(penta-sulfanilic acid)phosphonitrilic-polyetherether ketone] proton exchange membrane material and a preparation method thereof. The proton exchange membrane material has the structural formula that sulfonated polyetherether ketone with medium sulfonation degree is taken as a matrix material in the proton exchange membrane material, the defects that the water absorption rate in the sulfonated polyether ether ketone (SPEEK) with high sulfonation degree and the composite membrane has low stability are overcome, and the composite membrane has a certain mechanical strength and high alcohol resistance. According to introduction of phosphonitrile three-membered ring, the thermal stability and oxidization resistance of the SPEEK membrane material are improved; according to introduction of aromatic amino benzene serving as a hydrophobic grouping, the alcohol resistance is improved, and the swelling action of water is reduced; moreover, according to introduction of lots of sulfonic acid groups through a chemical bond mode, the proton conductivity of the proton exchange membrane is improved, the physical loss of the sulfonic acid groups is avoided, and the service life of the membrane is prolonged.

Description

technical field [0001] The invention relates to a sulfonated poly[(penta-p-aminobenzenesulfonic acid) cyclotriphosphazene-ether ether ketone] proton exchange membrane material and a preparation method thereof. Background technique [0002] Proton exchange membrane (PEM), as the core component of direct methanol fuel cell (DMFC), has received extensive attention and has become the focus of research work. It mainly plays the role of isolating fuel and conducting protons. Its performance directly determines the performance of fuel cells develop. [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 alcohol resistance in DMFC limit the further application of perfluorosulfonic acid membranes in fuel cells, and it is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L61/16C08G8/28C08J5/22H01M8/02
CPCY02E60/50
Inventor 郭强钱君质李夏张天骄童彤陈艺玮谭孝林
Owner SHANGHAI UNIV
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