Functional perfluoro resin and preparation method thereof

A functional and fluororesin technology, which is applied in the field of multi-component copolymerized perfluorinated ion exchange resin and its preparation, can solve the problem of insufficient molecular weight of the resin

Active Publication Date: 2010-07-14
SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is also to solve the problem that the molecular weight of the obtained resin is not high enough due to the chain transfer reaction of the short side group sulfonyl fluoride alkenyl ether monomer in the polymerization process

Method used

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  • Functional perfluoro resin and preparation method thereof
  • Functional perfluoro resin and preparation method thereof
  • Functional perfluoro resin and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0034] The preparation method of the functional perfluororesin with sulfonyl fluoride and sulfonate side groups is an emulsion polymerization reaction carried out in the water phase, and the steps are:

[0035] 1), after cleaning the reaction kettle, add pure water, sulfonyl fluoride pendant alkenyl ether and sulfonyl fluoride pendant alkenyl ether, the overall mass percentage concentration of the two sulfonyl fluoride pendant alkenyl ethers in water is 5-50 %, the overall mass percent concentration of the two sulfonate pendant alkenyl ethers in water is 0.5 to 5%;

[0036] 2) Fill the reaction kettle with tetrafluoroethylene monomer through the gas metering tank to a pressure of 2-10MPa;

[0037] 3) The temperature of the reactor is raised to 10-60°C, adding an initiator into the reaction system through a metering pump to initiate the reaction, and continuously adding tetrafluoroethylene monomer and initiator to the reactor to keep the reaction pressure of the reactor at 2-10...

specific Embodiment approach

[0049] The following examples are further illustrations of the present invention, but the present invention is not limited thereto. Unless otherwise specified, the reaction kettles used in each embodiment are all 10L stainless steel high-pressure reaction kettles, and are equipped with temperature sensors, pressure sensors, heating circulation systems, cooling circulation systems, stirring motors, internal cooling water pipes, liquid metering pumps, gas Feed valve, liquid feed valve, material discharge valve in the reactor.

[0050] The perfluoroalkyl initiator used in the synthesis process of the present invention can be prepared according to known techniques in the art, and the recommended preparation method of the present invention can be found in J.Org.Chem., 1982, 47(11):2009-2013.

[0051] Potassium persulfate, ammonium persulfate, N 2 f 2 All gases are available for purchase.

[0052] The comonomer tetrafluoroethylene, sulfonyl fluoride side group vinyl ether monomer...

Embodiment 1

[0053] Embodiment 1, (r=2)

[0054] Reactor is cleaned and adds 5.0L deionized water, 500ml contains 70g cerium sulfonate pendant vinyl ether monomer (1 ') ((F 2 C=CF-O-CF 2 CF 2 -SO 3 - ) 4 Ce 4+ ) and 25g cerium sulfonate pendant vinyl ether monomer (2') ((F 2 C=CF-O-CF 2 -CF(CF 3 )-O-CF 2 CF 2 -SO 3 - )3Ce 3+ ) aqueous solution, start the stirring device, vacuumize and replace with high-purity nitrogen for three times, after the oxygen content in the reactor is tested to be below 1ppm, vacuumize, and add 500g of sulfonyl fluoride pendant alkenyl ether into the reactor through the liquid feed valve Monomer(1)(F 2 C=CF-O-CF 2 -CF 2 -SO 2 F) and 500g sulfonyl fluoride pendant vinyl ether monomer (2) (F 2 C=CF-O-CF 2 -CF(CF 3 )-O-CF 2 CF 2 -SO 2 F) After that, fill the reaction kettle with tetrafluoroethylene monomer to a pressure of 2.3MPa, raise the temperature to 25°C, and add 2.2g perfluorobutyryl compound (CF 3 CF 2 CF 2 CO-OO-CCF 2 CF 2 CF 3 )...

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Abstract

The invention provides a functional perfluoro resin with sulfuryl fluoride and sulphonate lateral-group, belonging to the field of fluorine-containing high molecular materials. The functional perfluoro resin is prepared by multiply copolymerizing tetrafluoroethylene, two sulfuryl fluoride lateral-group vinyl ether monomers of different structures, two sulphonate lateral-group vinyl ether monomers which are respectively correspond to the sulfuryl fluoride lateral-group vinyl ether monomers of different structures, wherein the total mole fraction of the tetrafluoroethylene is 50-90.9 percent of a copolymer, the total mole fraction of the sulfuryl fluoride lateral-group vinyl ether monomers is 8.8-49.99 percent, and the total mole fraction of the sulphonate lateral-group vinyl ether monomers is 0.01-0.3 percent. A perfluoro ion exchange membrane prepared by the functional perfluoro resin not only has chemical mediator resistance, but also has high conductivity, mechanical strength and dimension stability, low membrane resistance and long service life, and is suitable for fuel cells or chlor-alkali electrolytic cells. The invention also provides a preparation method and application of the functional perfluoro resin.

Description

technical field [0001] The invention belongs to the field of fluorine-containing polymer materials, and relates to a functional fluororesin with ion exchange function and a synthesis method thereof, in particular to a multi-component copolymerized perfluorinated ion-exchange resin with sulfonyl fluoride and sulfonate side groups and its Preparation. Background technique [0002] Since DuPont processed perfluorosulfonic acid resins into perfluorosulfonic acid ion exchange membranes in the 1970s and this membrane was used in the chlor-alkali industry and proton exchange membrane fuel cells, perfluorosulfonic acid ion exchange resins have been widely used in countries all over the world. has been extensively studied. [0003] Fluorine-containing ion-exchange membranes containing ion-exchange groups, especially sulfonic acid groups and carboxylic acid groups, are more suitable for use as ion-exchange membranes for fuel cells and chlor-alkali electrolyzers due to their resistanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/26C08F216/14C08F2/26H01M8/02H01M2/16C25B1/46C25B13/08
CPCY02E60/12Y02E60/50Y02P70/50
Inventor 张永明秦胜高自宏魏茂祥王丽王汉利
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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