Suspension polymerization preparation method of perfluorinated sulfonic acid resin

A perfluorosulfonic acid resin, suspension polymerization technology, applied in the field of fuel cells, can solve the problems of high conductivity, difficult oxygen permeability, etc., and achieve the effects of high conductivity, high affinity, and improved solubility

Pending Publication Date: 2022-03-22
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN107075291A discloses a liquid composition for proton exchange membrane, which contains carrying-SO 3 Polymers of H contain at least one -SO 3 Z group (Z is H, alkali metal ion or NH 4+ ) and recurring units derived from at least one ethylenically unsaturated fluorinated monomer (B), the monomer (B) being optionally selected from the group consisting of Oxole, but there is no sulfonyl functional group on it, so it is difficult to maintain high conductivity while greatly improving oxygen permeability

Method used

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  • Suspension polymerization preparation method of perfluorinated sulfonic acid resin
  • Suspension polymerization preparation method of perfluorinated sulfonic acid resin
  • Suspension polymerization preparation method of perfluorinated sulfonic acid resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The reaction kettle was cleaned and dried and evacuated nitrogen-replacement until the moisture was 10 ppm or less, and the oxygen content was 10 ppm or less. Vacuzzing tetrafluoroethylene monomer to 0.1 MPa, then evacuate to 0.0001 MPa, then 300g deionized water, 90g monomer CF 2 = Cfocf 2 CF (CF 3 OCF 2 CF 2 SO 2 F and 25 g of monomer C, 3 g of hydroxymethylcellulose addition in the reactor, warmed to 60 ° C, pentafluoroethylene to the pressure of 2 MPa, 10 ml of 10 ml containing 0.1 g of peroxide diisopropyl carbonate with metering pump ( IPP) initiator solution, maintaining the reaction pressure at 2 MPa, and continuous additional 45g monomer CF 2 = Cfocf 2 CF (CF 3 OCF 2 CF 2 SO 2 F and 8.5 g of monomer C, when Tetrafluoro ethylene is added to 100 g, stopping the addition, allowing the reaction to continue, and the reaction is stopped, and the unreacted tetrafluoroethylene monomer is stopped. The material was discharged and transferred to a glass flask, and 5 times was...

Embodiment 2

[0035] The reaction kettle was cleaned and dried and evacuated nitrogen-replacement until the moisture was 10 ppm or less, and the oxygen content was 10 ppm or less. Vacuzzing tetrafluoroethylene monomer to 0.1 MPa, then evacuate to 0.0001 MPa, then 300 g of deionized water, 13.5 g of monomer CF 2 = Cfocf 2 CF (CF 3 OCF 2 CF 2 SO 2 F, 8.4GCF 2 = Cfocf 2 CF 2 SO 2 F and 51G monomer C, 3G methylcellulose addition in the reaction kettle, warmed to 30 ° C, transfer Tetrafluoroethylene to the pressure to 1 MPa, add 10 ml of 10 ml of 0.04 g of peroxide compound (CF) with metering pump (CF) 3 CF 2 CF 2 Co-oo-ccf 2 CF 2 CF 3The initiator solution, maintaining the reaction pressure around 1 MPa, and continuously supplement 56g monomer CF 2 = Cfocf 2 CF 2 SO 2 F and 0.5 g of monomer C, when Tetrafluoro ethylene is added to 100 g, stopping the addition, allowing the reaction to continue, and the reaction is stopped, the reaction is stopped, and the unreacted tetrafluoroethylene monomer is re...

Embodiment 3

[0037] The reaction kettle was cleaned and dried and evacuated nitrogen-replacement until the moisture was 10 ppm or less, and the oxygen content was 10 ppm or less. Vacuzzing tetrafluoroethylene monomer to 0.1 MPa, then evacuate to 0.0001 MPa, then 300 g of deionized water, 280g monomer CF 2 = Cfocf 2 CF 2 SO 2 F and 8.5 g of monomer C, 5 g of polyvinyl alcohol were added to the reactor, warmed to 100 ° C, and the addition of tetrafluoroethylene to the pressure reached 5 MPa to stop addition of tetrafluoroethylene, add 10 ml of 10 ml of 0.01 g of peroxide. Butyl compound (CF 3 CF 2 CF 2 Co-oo-ccf 2 CF 2 CF 3 ) And 0.01 g of cyclohexane initiator and chain transfer agent solution begin to react, continuous addition of 2.8 g of monomer CF 2 = Cfocf 2 CF 2 SO 2 F and 21G monomer C. When the pressure is reduced to 1 MPa, the reaction is stopped, and the unreacted tetrafluoroethylene monomer is recovered. The material was discharged and transferred to a glass flask, and the emulsion w...

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Abstract

The invention discloses a suspension polymerization preparation method of perfluorinated sulfonic acid resin, which comprises the following steps: by taking tetrafluoroethylene A, a monomer B containing a sulfonyl fluoride end group and a monomer C containing a sulfonyl fluoride end group as comonomers, pre-adding deionized water, the monomer B, the monomer C, a dispersing agent and an auxiliary agent into a reactor, replacing until the oxygen content is qualified, adding a catalyst, and reacting for 2-4 hours to obtain the perfluorinated sulfonic acid resin. Stirring is started, tetrafluoroethylene monomers are introduced, an initiator is added to initiate a polymerization reaction, comonomers are supplemented in the reaction process, and finally the sulfonyl fluoride type perfluorinated sulfonic acid resin is obtained. Wherein the structural formula of the monomer B is CF2 = CFO [CF2CF (CF3) O] a [CF2CF2] bSO2F, a is an integer from 0 to 1, and b is an integer from 1 to 2; the structural formula of the monomer C is as follows: the perfluorosulfonic acid resin disclosed by the invention further comprises a fluorine-containing cyclic monomer unit containing a perfluoroalkoxy group of an ether bond and a sulfonyl fluoride group, so that the processability in a general solvent is improved, and the perfluorosulfonic acid resin is high in conductivity and oxygen permeability. The suspension polymerization method has the advantages of stable molecular weight and distribution of the product, simple post-treatment process and low production cost.

Description

Technical field [0001] The present invention relates to the field of fuel cells, and more particularly to a suspension polymer preparation method of a perfluorosulfonic acid resin. Background technique [0002] The perfluorosulfonic acid resin was first developed by DuPont in the 1970s, and processed into a perfluorosulfonic acid proton exchange membrane, mainly in the modern chlor-alkali industry and fuel cell field. The electrolytic diaphragm composite the perfluorosulfonic acid resin and the perfluorocarboxylic acid resin showed its durability and efficiency, while the proton exchange membrane fuel cell showed great potential. [0003] Relevant patents and reports have been related to the study and preparation of perfluorosulfonic acid resin. CN107075291A discloses a liquid composition for a proton exchange membrane, wherein-SO is included 3 The polymer of H contains at least one-SO 3 Z group (Z is H, alkali metal ion or NH 4+ The repeating unit of the ethylenically unsaturate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/26C08F234/02C08F216/14C08F2/18C08F2/20C08F6/24C08L27/18
CPCC08F214/262C08F2/18C08F2/20C08F6/24C08F234/02C08F216/1475C08L27/18
Inventor 邵春明陈振华郦聪周晓勇方绍锋肖艳茹赵洁
Owner JUHUA GROUP TECH CENT
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