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A kind of perfluorosulfonic acid ion exchange membrane and its preparation method and application

A technology of perfluorosulfonic acid ions and perfluorosulfonic acid ethers, which is applied in the fields of final product manufacturing, sustainable manufacturing/processing, electrochemical generators, etc., and can solve problems such as poor ion selectivity, wide molecular weight distribution, and complex synthesis processes , to achieve good ion selectivity, excellent mechanical properties, and simple preparation process

Active Publication Date: 2021-08-24
DALIAN RONGKE POWER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of perfluorosulfonic acid resins is mentioned in the above patents, and there are many similar patent documents. In 1966, Connolly, a scientist from DuPont, USA, proposed the use of monomers such as perfluorosulfonyl vinyl ether and tetrafluoroethylene. The method of copolymerization prepares perfluorosulfonic acid resins, and these resins are all carried out under high temperature (usually greater than 200°C) and high pressure (~20MPa) using common free radical (co)polymerization methods, so it is inevitable to make the synthesized perfluorosulfonic acid resin The molecular weight distribution of sulfonic acid resin is wide, and the controllability becomes poor. For polymers, the wide molecular weight distribution means that the molecular weight of the components is different, and the distribution of molecular chain length is uneven. Under the same conditions, the crystallization efficiency will be inconsistent. , it is difficult to form relatively regular crystals, and the uniformity is poor, resulting in a significant decrease in its mechanical properties, which in turn has an adverse effect on the performance of perfluorosulfonic acid ion exchange membranes
[0003] At present, the membrane materials used at home and abroad are mainly Nation series membranes developed by DuPont of the United States. Nation membranes have excellent performance in terms of electrochemical performance and service life. The all-vanadium redox flow battery is specially developed and manufactured, so it has the disadvantage of poor ion selectivity, which limits the further industrial application of the membrane in the field of flow energy storage batteries

Method used

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  • A kind of perfluorosulfonic acid ion exchange membrane and its preparation method and application
  • A kind of perfluorosulfonic acid ion exchange membrane and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 138.6g (0.3mol) of perfluoro[2-(1-fluorosulfonylethoxy)-propyl vinyl ether] monomer, 0.943g (3.33mmol) of 1-cyano-1-phenylethyl di Thiophenyl ester (CDB), 0.182g (1.11mmol) azobisisobutyronitrile and 1.632g (6mmol) sodium dodecylsulfonate were dispersed into 1386g water under strong mechanical stirring, and the reaction system was removed Oxygen-inert gas operation, react at 80°C for 18h, then add 1.55g (5.00mmol) perfluorodivinylbenzene, continue stirring for 30min, add 5.468g (33.3mmol) azobisisobutyronitrile, continue stirring 2h, cool down, pass the air, stop the reaction;

[0031] The cooled reaction system was centrifuged to remove the supernatant, the lower layer was washed three times with deionized water, and then washed three times with DMSO to remove impurities such as residual monomers and water in the sample, and then the obtained sample was transferred to a three-port circle. Add DMSO solvent to the bottom flask, and heat at 120°C under the protection of ...

Embodiment 2

[0035] The difference between this example and Example 1 is that the amount of perfluoro[2-(1-fluorosulfonylethoxy)-propyl vinyl ether] monomer is changed to 277.2g (0.60mol) and dodecyl The amount of sodium sulfonate was changed to 3.264g (12mmol), the quality of deionized water was changed to 2772g, the reaction time was 24h, and a perfluorosulfonic acid ion exchange membrane with a thickness of 50±2μm was obtained.

[0036] In this example, perfluoro[2-(1-fluorosulfonylethoxy)-propyl vinyl ether]:chain transfer agent=180:1; perfluorodivinylbenzene:chain transfer agent=1.5:1 .

Embodiment 3

[0038] The difference between this example and Example 1 is that the amount of perfluoro[2-(1-fluorosulfonylethoxy)-propyl vinyl ether] monomer is changed to 462g (1.00mol) and dodecylsulfonate The amount of sodium acid was changed to 5.439g (20mmol), the quality of deionized water was changed to 4620g, and the reaction time was 30h to obtain a perfluorosulfonic acid ion exchange membrane with a thickness of 50±2μm.

[0039] In this example, perfluoro[2-(1-fluorosulfonylethoxy)-propyl vinyl ether]:chain transfer agent=300:1; perfluorodivinylbenzene:chain transfer agent=1.5:1 .

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Abstract

The invention belongs to the field of polymer functional membrane materials, and in particular relates to a perfluorosulfonic acid ion exchange membrane and its preparation method and application. The invention adopts the method of emulsion polymerization to obtain the polymer with narrow molecular weight distribution through the polymerization reaction of the perfluorosulfonic acid ether monomer and the chain transfer agent, and the perfluorosulfonic acid ion exchange membrane is prepared by casting method. The perfluorosulfonic acid ion exchange membrane has narrow molecular weight distribution, controllable molecular weight, larger crystal area and crystallinity, good ion selectivity and excellent mechanical properties, and can be better applied in flow batteries. The preparation process of the perfluorosulfonic acid ion exchange membrane of the present invention is simple, the conditions are mild, and it is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of polymer functional membrane materials, and in particular relates to an ion exchange membrane for a liquid flow battery and a preparation method and application thereof. Background technique [0002] Since DuPont announced the invention patent of perfluorosulfonic acid ion exchange membrane US 4433082 in 1984, a lot of research work has focused on the use of perfluorosulfonic acid resin modification, compounding and process expansion to prepare perfluorosulfonic acid ion exchange membranes. Chinese patent CN 103044698B discloses a method of dissolving perfluorosulfonic acid resin in a low-toxicity and low-boiling point solvent, drying to obtain perfluorosulfonic acid resin powder, and then directly stirring and dissolving the powder in a high-boiling point solvent to make a high-solid content High-viscosity film-making liquid, and then perform film-making operation; Chinese patent CN 102336924B discloses a method of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J5/18C08L29/10C08F216/14C08F212/34C08F2/38H01M8/18
CPCC08F2/38C08F216/1466C08J5/18C08J2329/10C08F216/1475H01M8/1032H01M8/188C08F212/34Y02E60/50Y02P70/50
Inventor 李全龙张华民徐鹤英张涛
Owner DALIAN RONGKE POWER