Solution polymerization preparation method of perfluorinated sulfonic acid resin

A technology of perfluorosulfonic acid resin and solution, applied in the field of fuel cells, can solve the problems of difficulty in improving electrical conductivity and poor oxygen permeability of resins, and achieve improved processability, improved solubility, and high affinity. Effect

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

[0008] However, the alkyl ether end group vinyl ether monomer (A) does not contain sulfonyl fluoride end group functional groups, and the resin prepared after the introduction is difficult to improve electrical conductivity and has poor oxygen permeability.

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 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, and then vacuumize to 0.0001MPa, then add 300mL1H-perfluorohexane, 45g monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F, 56gCF 2 = CFOCF 2 CF 2 SO 2 F and 17g 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 0.02g 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 2F and 8.5g monomer C, when tetrafluoroethylene addition reaches 100g, stop adding, allow reaction to continue, when still internal pressure is reduced to 1MPa, stop reaction, reclaim unreacted tetrafluoro...

Embodiment 2

[0039] 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, and then vacuumize to 0.0001MPa, then add 300mL dichloropentafluoropropane, 27g monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 Add F and 51g monomer C into the reaction kettle, control the temperature to 20°C, feed tetrafluoroethylene until the pressure reaches 1MPa, and add 10mL initiator solution containing 0.1g diisopropyl peroxydicarbonate (IPP) with a metering pump , maintain the reaction pressure at about 1MPa, and continuously add 90g of monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F and 0.5g monomer C, when the tetrafluoroethylene addition reaches 100g, stop adding, allow reaction to continue, when still internal pressure is reduced to 0.2MPa, stop reaction, reclaim unreacted tetrafluoroethylene monomer. Release the material and transf...

Embodiment 3

[0041] 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 add 300mL1,1,2,2-tetrafluoroethyl-2,2,2-trifluoroethyl ether, 180g monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F and 8.5g of monomer C were added to the reaction kettle, the temperature was raised to 120°C, tetrafluoroethylene was introduced until the pressure reached 5MPa, and the addition of tetrafluoroethylene was stopped, and 10mL containing 0.01g perfluorobutyryl peroxide (CF 3 CF 2 CF 2 CO-OO-CCF 2 CF 2 CF 3 ) and 0.01g methanol initiator and chain transfer agent solution, and continuously add 4.5g monomer CF 2 = CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F and 21g of monomer C, when the pressure in the kettle was reduced to 1MPa, the reaction was stopped, and the unreacted tetrafluoroethylene monomer was recovere...

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Abstract

The invention discloses a solution polymerization preparation method of perfluorinated sulfonic 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 a fluorine-containing solvent and the comonomers into a reactor, performing heating to 20-120 DEG C at a pressure of 0.2-5 MPa, adding an initiator to initiate a polymerization reaction, and supplementing the comonomers in the reaction process so as 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 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 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 solution polymerization method is low in dangerousness, and the molecular weight and molecular weight distribution of the product are easy to adjust.

Description

technical field [0001] The invention relates to the technical field of fuel cells, in particular to a solution polymerization preparation method of a perfluorosulfonic acid resin. Background technique [0002] Proton membrane fuel cell is a new type of fuel cell. Its electrolyte is a solid organic membrane. Under humidification, the membrane can conduct protons. It generally uses platinum as a catalyst, and the working environment temperature is generally 60°C-80°C. It is a low-temperature fuel cell. The proton exchange membrane fuel cell unit is mainly composed of a membrane electrode, a sealing ring, and a flow field plate with an air guide channel. The membrane electrode is the core part of the proton exchange membrane fuel cell. The membrane, that is, the proton exchange membrane, this membrane does not conduct electrons and is an excellent conductor of hydrogen ions. It not only serves as an electrolyte to provide a channel for hydrogen ions, but also serves as a diaphr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/26C08F216/14C08F234/02C08F2/06
CPCC08F214/262C08F2/06C08F216/1475C08F234/02
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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