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Bulk polymerization preparation method of perfluorinated sulfonic acid resin

A perfluorosulfonic acid resin, bulk polymerization technology, applied in the field of fuel cells, can solve the problems of difficult market promotion, high price, difficulty in synthesizing monomer A, etc., and achieves improved solubility, high affinity, improved The effect of machinability

Pending Publication Date: 2022-02-25
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The film property that this perfluorosulfonic acid resin prepares is better, but replace the tetrafluoroethylene monomer in the conventional perfluorosulfonic acid resin with monomer A, monomer A synthesis difficulty is very expensive, and the price is nearly that of tetrafluoroethylene Thousand times, it is difficult to market promotion

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] After cleaning and drying the reactor, vacuumize and replace with nitrogen until the water content is below 100ppm and the oxygen content is below 10ppm. Vacuumize and fill the tetrafluoroethylene monomer to 0.1MPa, then vacuumize to 0.0001MPa, and then fill 180g monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F, 168gCF 2 = CFOCF 2 CF 2 SO 2 F and 68g of monomer C were added to the reaction kettle, the temperature was raised to 60°C, tetrafluoroethylene was introduced until the pressure reached 2MPa, and 10mL containing 0.01g of perfluorobutyryl peroxide (CF 3 CF 2 CF 2 CO-OO-CCF 2 CF 2 CF 3 ) initiator solution, maintain the reaction pressure at about 2MPa, and continuously add 45g monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F and 8.5g monomer C, when the tetrafluoroethylene addition reaches 100g, stop adding, allow reaction to continue, when still internal pressure is reduced to 1MPa, stop reaction, reclaim unreacted tetrafluoroethylene monomer....

Embodiment 2

[0036] After cleaning and drying the reactor, vacuumize and replace with nitrogen until the water content is below 100ppm and the oxygen content is below 10ppm. Vacuumize and fill tetrafluoroethylene monomer to 0.1MPa, then vacuumize to 0.0001MPa, then fill 450g monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 Add F and 21g of monomer C into the reactor, raise the temperature to 30°C, feed tetrafluoroethylene until the pressure reaches 1MPa, add 10mL of initiator solution containing 0.05g of diisopropyl peroxydicarbonate (IPP) with a metering pump, Maintain the reaction pressure at about 1MPa, and continuously add 4.5g monomer CF2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F and 8.5g monomer C, when the tetrafluoroethylene addition reaches 100g, stop adding, allow reaction to continue, when still internal pressure is reduced to 0.5MPa, stop reaction, reclaim unreacted tetrafluoroethylene monomer. Release the material and transfer it to a glass flask, separate the solid and li...

Embodiment 3

[0038] After cleaning and drying the reactor, vacuumize and replace with nitrogen until the water content is below 100ppm and the oxygen content is below 10ppm. Vacuumize and fill the tetrafluoroethylene monomer to 0.1MPa, then vacuumize to 0.0001MPa, and then fill 134g monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F and 255g of monomer C were added to the reaction kettle, the temperature was raised to 100°C, tetrafluoroethylene was introduced until the pressure reached 5MPa, and the addition of tetrafluoroethylene was stopped, and 10mL containing 0.005g perfluorobutyryl compound (CF 3 CF 2 CF 2 CO-OO-CCF 2 CF 2 CF 3 ) and 0.01g cyclohexane initiator and chain transfer agent solution, and continuously add 90g monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F and 0.5g monomer C, when the pressure in the kettle was reduced to 1MPa, the reaction was stopped, and the unreacted tetrafluoroethylene monomer was recovered. Release the material and transfer it to a gl...

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Abstract

The invention discloses a bulk polymerization preparation method of perfluorosulfonic acid resin. The method comprises the following steps: taking tetrafluoroethylene A, a monomer B containing a sulfonyl fluoride terminal group and a monomer C containing a sulfonyl fluoride terminal group as comonomers, pre-adding the comonomers into a reactor, performing heating to 30-100 DEG C at a pressure of 0.5-5MPa, adding an initiator to initiate a polymerization reaction, and supplementing the comonomers in the reaction process to finally obtain the sulfonyl fluoride type perfluorinated sulfonic acid resin. The structural formula of the monomer B is CF2 = CFO[CF2CF(CF3)O]a[CF2CF2]bSO2F, wherein the a is an integer from 0 to 1, and the 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 both ether bond perfluoroalkoxy and sulfuryl fluoride groups, so that the processability of the resin in a general solvent is improved, and the resin is high in conductivity and oxygen permeability. The perfluorinated sulfonic acid resin with low hydrogen permeability is provided for proton exchange membrane application in a fuel cell or high oxygen permeability is provided for electrode application. The bulk polymerization method is high in reaction rate, simple to operate, low in production cost and pure in product.

Description

technical field [0001] The invention relates to the technical field of fuel cells, in particular to a bulk polymerization preparation method of a perfluorosulfonic acid resin. Background technique [0002] Perfluorosulfonic acid resins are mainly used in the modern chlor-alkali industry and the field of fuel cells. The electrolytic diaphragm composed of perfluorosulfonic acid resin and perfluorocarboxylic acid resin has shown its durability and high efficiency, and it has shown great potential in proton exchange membrane fuel cells. [0003] Related patents and reports have appeared in the research and preparation of perfluorosulfonic acid resins. CN103270008A discloses a functionalized perfluorodioxole or perfluorodioxolane monomer (A) having a fluoroalkylsulfonyl group, a fluoroalkylsulfonate group or a fluoroalkylsulfonic acid side group. Ionomer of polymerized units of fluoroolefin monomer (B) and ion-conductive composition formed therefrom, ion-conductive composition ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/26C08F216/14C08F234/02C08F2/02
CPCC08F214/262C08F216/1475C08F234/02C08F2/02
Inventor 邵春明郦聪陈振华周晓勇宝志超肖艳茹赵洁
Owner JUHUA GROUP TECH CENT
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