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Perfluorinated ion exchange resin and preparation method thereof

A technology of exchange resin and perfluorinated ion, which is applied in the field of perfluorinated ion exchange resin and its preparation, to achieve the effects of wide applicability, high conductivity and high mechanical strength

Active Publication Date: 2013-02-20
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

For example, US5654109, US5246792 and other patents disclose the use of double-layer material composite membranes to meet the requirements of high electrical conductivity and high strength at the same time, but there are still certain defects in the uniformity of ion conduction and the improvement of electrical conductivity.

Method used

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  • Perfluorinated ion exchange resin and preparation method thereof
  • Perfluorinated ion exchange resin and preparation method thereof
  • Perfluorinated ion exchange resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: a kind of preparation method of perfluorinated ion exchange resin, the steps are as follows:

[0038] Prepare precursor resin:

[0039] Wash the 10L reactor and add 6L of deionized water, 100ml of an aqueous solution containing 8g of ammonium perfluorooctanoate, 100ml of a sodium borate solution with a mass concentration of 3%, start the stirring device, and replace it three times. After testing, the oxygen content in the reactor is qualified (less than 5ppm ), vacuumize, and add 500g of sulfonyl fluoride pendant vinyl ether monomer 1 (structural formula: CF 2 =CF-O-CF 2 -CF 2 -SO 2 F) and 500g sulfonyl fluoride pendant vinyl ether monomer 2 (structural formula is: CF 2 =CF-OCF 2 -CF(CF 3 )-O-CF 2 CF 2 SO 2 After F), fill the reaction kettle with tetrafluoroethylene monomer and keep the pressure to 2.3MPa, raise the temperature to 65°C, add 100g of ammonium persulfate aqueous solution (initiator solution) with a mass concentration of 3% with a met...

Embodiment 2

[0046] Embodiment 2: a kind of preparation method of perfluorinated ion exchange resin comprises the following steps:

[0047] Prepare the precursor resin with sulfonyl fluoride side group according to the method of embodiment 1, the difference is: add 600g sulfonyl fluoride monomer 1 (CF 2 =CF-O-CF 2 CF 2 -SO 2 F) and 300 g of sulfonyl fluoride monomer 2 (CF 2 =CF-O-CF 2 CF (CF 3 )-O-CF 2 CF 2 SO 2 F), and maintain a reaction pressure of 1.8MPa for polymerization reaction to obtain a precursor resin.

[0048] Precursor resin data:

[0049] by F 19 NMR and IR analysis confirmed that it was a ternary polymer. According to the integrated value of fluorine NMR, the molar percentage of tetrafluoroethylene contained in the polymer structure was 58.1%. 2 =CF-O-CF 2 -CF 2 -SO 2 F) The molar percentage is 33.4%, containing sulfonyl fluoride group enyl ether monomer (CF 2 =CF-OCF 2 -CF(CF 3 )-O-CF 2 CF 2 SO 2 F) The mole percentage is 8.5%, in the overall resin -SO ...

Embodiment 3

[0054] Embodiment 3: a kind of preparation method of perfluorinated ion exchange resin comprises the following steps:

[0055]Clean the reactor and add 6L of deionized water, 100ml of an aqueous solution containing 10g of sodium dodecylsulfonate, start the stirring device, vacuumize, and replace with high-purity nitrogen for three times. After testing, the oxygen content in the reactor is below 10ppm , vacuumize, add 1000g sulfonyl fluoride pendant vinyl ether monomer 1 (CF 2 =CF-O-CF 2 -CF 2 -SO 2 After F), fill the reaction kettle with tetrafluoroethylene monomer pressure to 2.0MPa, raise the temperature to 55°C, and add 100g of azodibutylamidine hydrochloride aqueous solution (initiator solution) with a mass concentration of 4.5% with a metering pump , to initiate the polymerization reaction, continue to feed tetrafluoroethylene monomer to keep the reaction pressure at 2.0MPa, add 30g of initiator solution to the system every 30min, stop adding the initiator after reacti...

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Abstract

The invention provides a perfluorinated ion exchange resin and a preparation method thereof. The perfluorinated ion exchange resin has a structure shown in a formula (I). The preparation method of the perfluorinated ion exchange resin comprises the following step: performing complete or partial grafting reaction on a precursor resin and a functional monomer under certain conditions. The perfluorinated ion exchange resin synthesized by the invention can simultaneously meet the requirements for high ion exchange capacity and large mechanical strength, and has wide applicability; and by regulating the ratio of the functional monomer in the raw materials, perfluorinated ion exchange resins which have different ion exchange capacities and mechanical properties to meet various requirements can be prepared.

Description

technical field [0001] The invention belongs to the technical field of fluorine-containing polymer materials, and relates to a perfluorinated ion-exchange resin with high exchange capacity and a preparation method thereof, in particular to a perfluorinated ion-exchange resin with a perfluorosulfonimide group in the side chain Resins and methods for their preparation. Background technique [0002] Since DuPont processed perfluorosulfonic acid resins into perfluorosulfonic acid ion exchange membranes in the 1970s and applied the membranes in the chlor-alkali industry and proton exchange membrane fuel cells, perfluorinated ion exchange resins have been widely used in countries all over the world. Extensive research. [0003] Perfluorinated ion-exchange membrane materials are suitable for electrochemical separators due to their stable chemical degradation resistance and ion conductivity. US3282875 is the first document published by DuPont about the synthesis of sulfonyl fluori...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F214/26C08F216/14C08F8/32B01J39/20
Inventor 王丽张永明滕培峰王凯
Owner SHANDONG DONGYUE WEILAI HYDROGEN ENERGY MATERIAL CO LTD
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