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Preparation method of perfluorinated sulfonic acid resin solid

A perfluorosulfonic acid resin and solid technology, which is applied in the field of preparation of perfluorosulfonic acid resin solids, can solve the problems of large sewage, limited cleaning effect of water washing, and difficulty in removing lipophilic and hydrophobic impurities.

Active Publication Date: 2021-12-07
国家电投集团氢能科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The limitations of washing with water are: (1) perfluorosulfonic acid resin has strong adsorption to some impurities, and the cleaning effect of water washing is limited; (2) it is difficult to remove lipophilic and hydrophobic impurities; Yield; (4) will produce a large amount of sewage
Therefore, the solid crystallinity obtained by using the perfluorosulfonic acid resin dispersion liquid dried at high temperature is high, and it is difficult to redissolve, and the application is limited.
[0014] Therefore, it is necessary to develop a method for preparing a solid perfluorosulfonic acid resin to solve the problems of solid preparation, purification, and difficulty in dissolving and dispersing crystalline polymers in liquid solvents during the production and recycling of perfluorosulfonic acid resins.

Method used

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  • Preparation method of perfluorinated sulfonic acid resin solid
  • Preparation method of perfluorinated sulfonic acid resin solid
  • Preparation method of perfluorinated sulfonic acid resin solid

Examples

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preparation example Construction

[0062] A kind of preparation method of perfluorosulfonic acid resin solid of the embodiment of the present invention, comprises:

[0063] a, dispersing the perfluorosulfonic acid resin in a solvent to obtain a perfluorosulfonic acid resin dispersion;

[0064] b. Add the perfluorosulfonic acid resin dispersion obtained in step a into an organic precipitant, precipitate and filter to obtain a solid product, and the organic precipitant is selected from the first precipitant, the second precipitant or the third precipitant At least one of the agents, wherein, the first precipitation agent is selected from carbon five alkanes, carbon six alkanes, carbon seven alkanes, carbon eight alkanes, carbon nine alkanes, carbon ten alkane, perfluoro-n-hexane or petroleum ether At least one, the second precipitation agent is selected from carbon disulfide, methylene chloride, carbon tetrachloride, chloroform, ethyl chloride, C 2 h 4 Cl 2 、C 2 h 3 Cl 3 、C 3 h 7 Cl, C 4 h 9 Cl or C 5 ...

Embodiment 1

[0118] Example 1 Using different solvents to dissolve and disperse perfluorosulfonic acid resins to obtain solid perfluorosulfonic acid resins

[0119] Weigh 1 g of perfluorosulfonic acid resin A into 9 g of solvent, and dissolve under certain conditions to obtain a clear and transparent dispersion. The dispersion was added to 25 g of n-hexane to obtain a precipitate. The precipitate was vacuum-dried at 180 °C for 4 h, and the solid perfluorosulfonic acid resin was obtained after drying.

[0120] The structural formula of perfluorosulfonic acid resin A in the present embodiment is:

[0121]

[0122] Solvents used for resin dissolution and dispersion in this embodiment include water, methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, ethylene glycol, 1,2 propylene glycol, 1,3 propylene glycol, glycerol At least one of alcohol, N,N-dimethylformamide (DMF), N,N-dimethylacetamide (DMAc), dimethylsulfoxide (DMSO) and N-methylpyrrolidone (NMP).

[0123] In orde...

Embodiment 2

[0131] Embodiment 2: adopt the organic precipitant that contains the first precipitant to make perfluorosulfonic acid resin solid

[0132] Weigh 80 g of perfluorosulfonic acid resin B and put it into 320 g of solvent. The solvent used is dimethyl sulfoxide and isopropanol with a mass ratio of 1:2. Dissolve at 60 °C for 1 h under normal pressure. Obtained 400 g of clear and transparent dispersion liquid W. 5 g of dispersion W was added to 15 g of different types of precipitants to obtain precipitation. The precipitate was air-dried at 220 °C for 0.5 h, and the solid perfluorosulfonic acid resin was obtained after drying.

[0133] The structural formula of perfluorosulfonic acid resin B in the present embodiment is:

[0134]

[0135] The organic precipitant used in this embodiment includes the first precipitant, specifically n-pentane, n-hexane, cyclohexane, perfluoro-n-hexane, a mixture of two carbon hexanes, petroleum ether, industrial hexane, industrial heptane And the ...

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Abstract

The invention discloses a preparation method of a perfluorinated sulfonic acid resin solid, which comprises the steps of a, dispersing perfluorinated sulfonic acid resin in a solvent to obtain a perfluorinated sulfonic acid resin dispersion; b, adding the perfluorinated sulfonic acid resin dispersion obtained in the step a into an organic precipitant, separating out precipitation, and obtaining a solid product through filtration, wherein the organic precipitant is selected from at least one of a first precipitant, a second precipitant or a third precipitant, and the solvent and the precipitant in the step a are mutually soluble; and c, drying the solid product obtained in the step b to obtain the perfluorosulfonic acid resin solid. According to the method disclosed by the invention, the pure perfluorosulfonic acid resin solid can be obtained, the product purity can be improved in the production process, sewage generated in the fluorination industry is reduced, and the batch stability is improved.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a method for preparing a solid perfluorosulfonic acid resin. Background technique [0002] Perfluorosulfonic acid resin (PFSA), as an ion exchange resin, is a cutting-edge material in the fluorine material industry. Almost all commercially available perfluorosulfonic acid resins are based on DuPont's Nafion resin. In the 1960s, Nafion resin was used in polyelectrolyte diaphragms in the chlor-alkali industry. In the 1980s, it was applied to fuel cells by Canada's Ballard Company, which accelerated the development of fuel cell technology. At present, all the ion exchange membranes of vehicle fuel cells actually put into use are prepared on the basis of perfluorosulfonic acid resin. [0003] In addition to being used in the chlor-alkali industry and fuel cells, the ion exchange membranes prepared by perfluorosulfonic acid resins are also widely used in flow...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/26C08F6/12
CPCC08F6/12C08L27/18
Inventor 张泽天周朝毅刘昊李道喜李蕴熙董天都贾雯迪潘丹丹鹿传睿刘品阳王福瑶
Owner 国家电投集团氢能科技发展有限公司
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