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Ion exchange resin and preparation method thereof

The technology of ion exchange resin and tetrafluoroethylene is applied in the field of ion exchange resin and its preparation, and can solve the problems of low reactivity rate of sulfonyl fluoride-based vinyl ether monomer, low polymer yield, high requirement of reaction conditions and the like, To achieve the effect of increasing hydrophilic properties, simple preparation method and improving moisturizing properties

Pending Publication Date: 2022-04-19
国家电投集团氢能科技发展有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of copolymerization of fluorine-containing vinyl monomers and sulfonyl fluoride vinyl ether monomers, the reactivity rate of sulfonyl fluoride vinyl ether monomers is low, the requirements for reaction conditions are high, and the yield of polymers is low

Method used

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  • Ion exchange resin and preparation method thereof
  • Ion exchange resin and preparation method thereof
  • Ion exchange resin and preparation method thereof

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preparation example Construction

[0045] The embodiment of the present invention also provides a kind of preparation method of ion exchange resin, comprises the following steps:

[0046] a. Addition reaction of perfluoro β-ethane sultone or sulfonyl fluoride acetyl fluoride with perfluoropropylene oxide to obtain the addition product, whose molecular formula is FOC(CF(CF 3 )OCF 2 ) X CF 2 SO 2 F, where x is 1, 2 or 3;

[0047] B, carry out copolymerization reaction with allyl alcohol monomer and tetrafluoroethylene monomer, make tetrafluoroethylene-allyl alcohol copolymer;

[0048] c. Carry out graft reaction between the tetrafluoroethylene-allyl alcohol copolymer prepared in step b and the addition product obtained in step a, and transform to obtain an ion exchange resin.

[0049] The reaction formula of the embodiment of the present invention is as follows, taking X=1 as an example:

[0050]

[0051] The preparation method of the ion exchange resin of the embodiment of the present invention is to po...

Embodiment 1

[0062] Dehumidify and deoxygenate the reactor, the oxygen content does not exceed 10ppm, the water content does not exceed 10ppm, quickly add dry diethylene glycol dimethyl ether, KF, perfluoro β-ethane sultone, stir evenly, and heat up to 30°C , slowly feed metered dry perfluoropropylene oxide, wherein the molar ratio of perfluoropropylene oxide to perfluoro β-ethane sultone is 1.2:1, keep the pressure at 0.2Mpa, react for 8 hours, and refine the product Distillation to obtain adduct product A.

[0063] Add 58g of allyl alcohol, 9g of azobisisobutyronitrile, 90g of butyl acetate, and 90g of methyl isobutyl ketone into the reaction kettle, stir evenly, vacuumize, and inject N 2 , then evacuate, feed tetrafluoroethylene to the reactor pressure of 2.0MPa, raise the temperature to 68°C, react for 14 hours, stop the reaction when the reactor pressure is between 0.8-1.0MPa, collect unreacted tetrafluoroethylene gas and olefin The propanol monomer is purified to obtain a tetrafluor...

Embodiment 2

[0068] Dehumidify and deoxygenate the reactor, the oxygen content does not exceed 10ppm, the water content does not exceed 10ppm, quickly add dry diethylene glycol dimethyl ether, KF, perfluoro β-ethane sultone, stir well, and heat up to 40°C , slowly feed metered dry hexafluoropropylene oxide, wherein the molar ratio of perfluoropropylene oxide to perfluoro β-ethane sultone is 1.3:1, keep the pressure at 0.3Mpa, react for 7 hours, and carry out rectification of the product , to obtain the one-time addition product A.

[0069] Add 87g of allyl alcohol, 9g of azobisisobutyronitrile, 90g of butyl acetate, and 90g of methyl isobutyl ketone into the reaction kettle, stir evenly, vacuumize, and introduce N 2 , then evacuate, feed tetrafluoroethylene to the reactor pressure of 2.0MPa, raise the temperature to 75°C, react for 16 hours, stop the reaction when the reactor pressure is between 0.9-1.0MPa, collect unreacted tetrafluoroethylene gas and alkene The propanol monomer is purif...

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Abstract

The invention discloses a preparation method of ion exchange resin, which comprises the following steps: a, perfluoro beta-ethane sultone or sulfonyl fluoride acetyl fluoride and perfluoropropylene oxide are subjected to addition reaction to prepare an addition product, the molecular formula of the addition product is FOC (CF (CF3) OCF2) XCF2SO2F, and x is 1, 2 or 3; b, carrying out a copolymerization reaction on an allyl alcohol monomer and a tetrafluoroethylene monomer to prepare a tetrafluoroethylene-allyl alcohol copolymer; and c, carrying out grafting reaction on the tetrafluoroethylene-allyl alcohol copolymer prepared in the step b and the addition product prepared in the step a, and transforming to obtain the ion exchange resin. According to the method disclosed by the invention, the defect of low reactivity rate of the sulfonyl fluoride vinyl ether monomer and the tetrafluoroethylene in the copolymerization process is effectively avoided; meanwhile, the problems that in the sulfonyl fluoride vinyl ether monomer preparation process, a five-membered ring reaction is easily formed in the salt forming and decarboxylation process, the complexity of the preparation process is increased, and the yield is reduced are solved.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to an ion exchange resin and a preparation method thereof. Background technique [0002] In 1962, the American DuPont Company (Du Pont) first developed the commercially known as The perfluorosulfonic acid ion polymer (PFSI, also known as perfluorosulfonic acid ion exchange resin), as a high polymer solid electrolyte with high chemical stability, is used in fuel cells developed by aerospace, creating a perfluoroionic polymer The first of its kind. [0003] In the existing literature reports, the preparation of fluorine-containing ion exchange resins mostly adopts the copolymerization of tetrafluoroethylene and sulfonyl vinyl ether monomers. Dow company disclosed in patent US4358545, US4940525 to adopt short side group monomer (sulfonyl fluoride vinyl ether, CF 2 = CFOCF 2 CF 2 SO 2 F) Copolymerize with fluorine-containing vinyl monomers such as tetrafluor...

Claims

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Application Information

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IPC IPC(8): C08F259/08C08F216/14C08F214/26C08F216/08
CPCC08F259/08C08F214/265C08F216/08C08F216/1475Y02E60/50
Inventor 王福瑶李道喜刘昊干志强方亮刘品阳刘飞王杰李震康夏丰杰刘真
Owner 国家电投集团氢能科技发展有限公司
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