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Preparation method of polysulfone cation-exchange membrane

An ion exchange membrane, polysulfone technology, applied in the field of sulfonated polysulfone, can solve problems such as being unsuitable for fuel cell applications

Active Publication Date: 2014-07-23
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, commercialized polysulfone-based cation exchange membranes are mostly main-chain membrane products made by direct sulfonation modification of polysulfone, which are mainly used for membrane separation and are not suitable for fuel cell applications.

Method used

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  • Preparation method of polysulfone cation-exchange membrane
  • Preparation method of polysulfone cation-exchange membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1:

[0045] (1) Bonding of ethyl isocyanate on the main chain of polysulfone skeleton: In a four-neck flask equipped with a stirrer and a thermometer, add 0.65g of polysulfone and 48mL of N,N-dimethylacetamide to make PSF Dissolve completely; then, under nitrogen protection, add 1.3 mL of chloroethyl isocyanate and 1.3 mL of anhydrous SnCl 4 , The Friedel-Crafts alkylation reaction between chloroethyl isocyanate and PSF macromolecular chains was carried out at 60°C for 24h, and a clear and transparent intermediate product solution was obtained.

[0046] (2) Preparation of sulfonated modified polysulfone: raise the temperature of the intermediate product solution to 100°C, add 5.00g of sodium p-hydroxybenzenesulfonate and 0.04g of dibutyltin dilaurate (catalyst), to make the PSF-eic chain The reaction of the isocyanate group on the above and the hydroxyl group of sodium p-hydroxybenzenesulfonate to form carbamate was carried out for 10 hours. After the reactio...

Embodiment 2

[0051] (1) Bonding of ethyl isocyanate on the main chain of polysulfone skeleton: In a four-neck flask equipped with a stirrer and a thermometer, add 0.66g of polysulfone and 49mL of N,N-dimethylacetamide to make PSF Dissolve completely; then, under nitrogen protection, add 1.35 mL of chloroethyl isocyanate and 1.35 mL of anhydrous SnCl 4 , The Friedel-Crafts alkylation reaction between chloroethyl isocyanate and PSF macromolecular chains was carried out at 65°C for 22h, and a clear and transparent intermediate product solution was obtained.

[0052] (2) Preparation of sulfonated modified polysulfone: raise the temperature of the intermediate product solution to 100°C, add 5.20g of sodium p-hydroxybenzenesulfonate and 0.05g of dibutyltin dilaurate (catalyst), to make the PSF-eic chain The reaction of the isocyanate group on the above and the hydroxyl group of sodium p-hydroxybenzenesulfonate to form carbamate was carried out for 12 hours. After the reaction, 200 mL of ethanol ...

Embodiment 3

[0056] (1) Bonding of ethyl isocyanate on the main chain of polysulfone skeleton: In a four-neck flask equipped with a stirrer and a thermometer, add 0.68g of polysulfone and 50mL of N,N-dimethylacetamide to make PSF Dissolve completely; then under nitrogen protection, add 1.38mL of chloroethyl isocyanate and 1.35mL of anhydrous SnCl 4 , The Friedel-Crafts alkylation reaction between chloroethyl isocyanate and PSF macromolecular chains was carried out at 70°C for 24h, and a clear and transparent intermediate product solution was obtained.

[0057] (2) Preparation of sulfonated modified polysulfone: raise the temperature of the intermediate product solution to 100°C, add 5.30g of sodium p-hydroxybenzenesulfonate and 0.04g of dibutyltin dilaurate (catalyst), to make the PSF-eic chain The reaction of the isocyanate group on the above and the hydroxyl group of sodium p-hydroxybenzenesulfonate to form carbamate was carried out for 13 hours. After the reaction, 200 mL of ethanol was...

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Abstract

The invention discloses a preparation method of a polysulfone cation-exchange membrane, relating to sulfonated polysulfone. The method comprises the following steps: (1) dissolving 0.65-0.7g of PSF in 48-55mL of N,N-dimethyl acetamide, adding 1.3-1.5mL of chloroethyl isocyanate and 1.3-1.5mL of anhydrous SnCl4, and reacting at 60-70 DEG C for 20-24 hours to obtain a transparent solution; (2) heating the transparent solution to 100 DEG C, adding 5.00-5.50g of sodium 4-hydroxybenzenesulfonate and 0.04-0.05g of dibutyltin dilaurate, reacting for 10-15 hours, adding 200mL of ethanol, separating, and alternately washing with distilled water and ethanol to obtain sulfonated modified polysulfone (PSF-sas); and (3) dissolving the PSF-sas in chloroform, running to form a film, and drying to remove the solvent, thereby obtaining the finished product. The preparation method is simple; and the product has higher degree of sulfonation and cation-exchange membrane properties, and can be used in proton-exchange membrane fuel batteries.

Description

technical field [0001] The invention relates to sulfonated polysulfone, in particular to a preparation method of polysulfone cation exchange membrane. Background technique [0002] Polymer electrolyte membrane (Polymer electrolyte membrane, PEM) is a key component of proton exchange membrane fuel cells and direct methanol fuel cells. The PEM can provide a fast channel for the transport of hydrogen ions from the anode to the cathode, while preventing the mixing of fuel gas and oxidant gas. At present, the commonly used proton exchange membrane is Nafion proton exchange membrane (perfluorosulfonic acid membrane) of DuPont Company of the United States. This exchange membrane has disadvantages such as high cost, inability to operate at high temperature, and high methanol permeability in direct methanol fuel cells. [0003] In order to promote the development of proton exchange membrane fuel cells, people are vigorously developing new high-performance and low-cost non-fluorine p...

Claims

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Application Information

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IPC IPC(8): C08J5/22C08L81/06C08G75/20H01M8/02H01M8/10H01M8/1027H01M8/1032
CPCY02E60/50
Inventor 杜瑞奎安富强高保娇李延斌
Owner ZHONGBEI UNIV
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