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Fluorine-containing amphiphilic block copolymer, preparation and application thereof, fluorine-containing amphiphilic block copolymer hybrid proton exchange membrane and preparation thereof

A proton exchange membrane and amphiphilic block technology, which is applied in the field of fluorine-containing amphiphilic block copolymer hybrid proton exchange membrane and its preparation, can solve the problems of difficult dispersion, difficult synthesis, poor compatibility, etc., and achieve Good compatibility, effect of improving dimensional stability

Active Publication Date: 2022-08-02
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the poor compatibility between inorganic components and carbon materials and polymers due to the high polar surface, and the size is much larger than the Nafion phase structure size, even the surface-modified inorganic components are still easy to aggregate in the Nafion film, which is difficult to evenly dispersed
Although the doping of polytetrafluoroethylene and other non-proton-conducting polymers enhances the mechanical strength, dimensional stability, ion selectivity and alcohol resistance of Nafion, it will lead to a decrease in its conductivity.
The method of covalent chemical modification and surface modification on Nafion has technical problems such as difficult synthesis and complicated operation

Method used

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  • Fluorine-containing amphiphilic block copolymer, preparation and application thereof, fluorine-containing amphiphilic block copolymer hybrid proton exchange membrane and preparation thereof
  • Fluorine-containing amphiphilic block copolymer, preparation and application thereof, fluorine-containing amphiphilic block copolymer hybrid proton exchange membrane and preparation thereof
  • Fluorine-containing amphiphilic block copolymer, preparation and application thereof, fluorine-containing amphiphilic block copolymer hybrid proton exchange membrane and preparation thereof

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preparation example Construction

[0033] The present invention provides the preparation method of the fluorine-containing amphiphilic block copolymer described in the above technical scheme, comprising the following steps:

[0034] Mix perfluoroalkyl alcohol, trifluoromethanesulfonic anhydride, auxiliary agent and first solvent, and carry out esterification reaction to obtain perfluoroalkyl trifluoromethanesulfonate; the structural formula of the perfluoroalkyl alcohol is F 3 C-(CF 2 -CF 2 ) m -(CH 2 -CH 2 ) n -OH; wherein, m=1~6, n=0.5~1;

[0035] The perfluoroalkyl trifluoromethanesulfonate, the oxazoline monomer and the second solvent are mixed, and ring-opening polymerization is carried out under anhydrous and oxygen-free conditions to obtain a fluorine-containing amphiphilic block copolymer; the oxazole The morpholine monomer is 2-methyl-2-oxazoline or 2-ethyl-2-oxazoline.

[0036] In the present invention, unless otherwise specified, the required preparation raw materials are all commercially availa...

Embodiment 1

[0077] Into a round-bottomed three-necked flask were added 1 g (2.16 mmol) of perfluoroalkyl alcohol, 0.36 mL (2.59 mmol) of dry triethylamine, 0.027 g (0.22 mmol) of 4-dimethylaminopyridine and 15 mL of dry dichloromethane , 0.435 mL (2.57 mmol) of trifluoromethanesulfonic anhydride was added dropwise under nitrogen protection, under the condition of ice-salt bath at -10 °C, and the dropwise addition process continued for 0.5 h; after the dropwise addition, the reaction was continued in the ice-salt bath environment for 40 min, and then removed Ice-salt bath, continue to react at 25°C for 12h;

[0078] After the reaction was completed, 10 mL of ice water was added to the reaction system to quench, and the liquids were separated, and the organic phase was collected and subjected to rotary evaporation under vacuum conditions. , to obtain the ether solution of the crude product; 20 mL of the ether solution of the crude product was washed with 10 mL of ice water each time, repeat...

Embodiment 2

[0084] Prepare perfluoroalkyl trifluoromethanesulfonate according to the method of embodiment 1;

[0085] Combine 0.3 g (0.50 mmol) of perfluoroalkyl trifluoromethanesulfonate with 0.865 mL (10 mmol) of 2-methyl-2-oxazoline monomer (oxazoline monomer and perfluoroalkyl trifluoromethanesulfonate) The molar ratio of oxazoline is 20:1), mixed with 1.65 mL of absolutely dry acetonitrile, so that the concentration of oxazoline monomer is 4 mol / L, under the protection of anhydrous and oxygen-free argon, after cationic ring-opening polymerization reaction is carried out in an oil bath at 80 °C for 10 h, the The reaction system was cooled to room temperature, and 7.5 mL of a methanol solution of 0.1 mol / L potassium hydroxide was added with a syringe. The molar ratio of potassium hydroxide to perfluoroalkyl trifluoromethanesulfonate was 1.5:1, under argon protection and room temperature conditions. to terminate for 4h;

[0086] After the termination, rotary evaporation was performed u...

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Abstract

The invention provides a fluorine-containing amphiphilic block copolymer, preparation and application thereof, a fluorine-containing amphiphilic block copolymer hybrid proton exchange membrane and preparation thereof, and belongs to the technical field of proton exchange membranes. The fluorine-containing segment of the block copolymer disclosed by the invention has good compatibility with a perfluorosulfonic acid membrane; the amide group of the polyoxazoline segment with the repeating unit containing the amide group in the block copolymer is hydrolyzed into a secondary amine group in the acidification process of the perfluorosulfonic acid membrane, and the secondary amine group and the sulfonic acid group of the perfluorosulfonic acid membrane are subjected to electrostatic interaction to realize crosslinking. The size stability of the perfluorosulfonic acid membrane is improved, and the perfluorosulfonic acid membrane is endowed with the potential of preventing cross permeation of fuel or electrolyte; a secondary amine group obtained after hydrolysis is a proton acceptor and can be used as an additional proton conduction site, so that the conductivity of the perfluorosulfonic acid membrane is not sacrificed. The fluorine-containing amphiphilic block copolymer provided by the invention improves the dimensional stability of a perfluorosulfonic acid membrane while not sacrificing the conductivity, so that the perfluorosulfonic acid membrane has greater potential when being used as a proton exchange membrane.

Description

technical field [0001] The invention relates to the technical field of proton exchange membranes, in particular to a fluorine-containing amphiphilic block copolymer and its preparation and application, a fluorine-containing amphiphilic block copolymer hybrid proton exchange membrane and its preparation. Background technique [0002] Proton exchange membrane is the core part of proton exchange membrane fuel cell, all-vanadium redox flow battery and other potential energy conversion and storage devices for stationary or portable electronic equipment and water electrolysis cells for producing clean energy. , which directly determines their performance. At present, the Nafion series of perfluorosulfonic acid membranes produced by DuPont have become the most widely used proton exchange membranes due to their good chemical stability, mechanical strength and high proton conductivity. [0003] However, Nafion film still suffers from poor dimensional stability and degradation of mec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/02H01M8/103H01M8/1067H01M8/1069
CPCC08G73/0233H01M8/103H01M8/1067H01M8/1069Y02P70/50Y02E60/50
Inventor 李昊龙翟靓
Owner JILIN UNIV
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