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Method for preparing P(VDF-DB)-g-S-C3H6-SO3H proton exchange membrane material

A proton exchange membrane and VDF-DB technology, which is applied in the field of preparing fluoropolymer-based proton exchange membrane materials, can solve the problems of complex preparation process and complex process, and achieve the effect of simple process and mild conditions.

Active Publication Date: 2018-01-09
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome problems such as complicated technique in the proton exchange membrane material preparation process, the object of the present invention is to provide a kind of preparation P(VDF-DB)-g-S-C by P(VDF-CTFE) by elimination and addition reaction 3 h 6 -SO 3 The method of H proton exchange membrane material, by using commercialized P (VDF-CTFE) as raw material, eliminates reaction with TEA under mild environment, and then undergoes thiolene addition reaction with sodium mercaptosulfonate to generate Graft polymer with high grafting amount of sodium sulfonate side chain
Treat the grafted polymer with acid to obtain a fluoropolymer containing a sulfonic acid group side chain, which solves the problem of complicated preparation process in the current method

Method used

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  • Method for preparing P(VDF-DB)-g-S-C3H6-SO3H proton exchange membrane material
  • Method for preparing P(VDF-DB)-g-S-C3H6-SO3H proton exchange membrane material
  • Method for preparing P(VDF-DB)-g-S-C3H6-SO3H proton exchange membrane material

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Experimental program
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Embodiment 1

[0026] This embodiment includes the following steps:

[0027] Step 1: Add the raw material P(VDF-CTFE) into the reaction bottle, and add the solvent N-methylpyrrolidone at the same time. After fully dissolving, add a sufficient amount of catalyst triethylamine, and stir the reaction at 55°C-65°C for 24 hours. The resulting polymer solution P(VDF-DB) was precipitated with deionized water, while excess triethylamine was removed with hydrochloric acid. After soaking the precipitated polymer in methanol, it is vacuum-dried to constant weight at no higher than 50°C. At this time, the structure can be characterized by nuclear magnetic resonance. The hydrogen nuclear magnetic resonance spectrum can be seen in figure 1 , it can be clearly seen that P(VDF-DB) has a new multiple peak at 6.1-6.5ppm than the raw material, and this peak corresponds to the chemical shift of (-CF2-CF=CH-CF2-)H on the double bond .

[0028] Step two:

[0029] Add the polymer P(VDF-DB) obtained in step 1 in...

Embodiment 2

[0037] This embodiment includes the following steps:

[0038] Step 1: Add the raw material P(VDF-CTFE) into the reaction bottle, and add the solvent at the same time. After fully dissolving, add a sufficient amount of catalyst triethylamine, and stir the reaction at 55°C-65°C for 24 hours. The resulting polymer solution P(VDF-DB) was precipitated with deionized water, while excess triethylamine was removed with hydrochloric acid. The precipitated polymer is soaked in methanol, and vacuum-dried to a constant weight at a temperature not higher than 50°C.

[0039] Step two:

[0040] Add the polymer P(VDF-DB) obtained in step 1 into the reaction flask, the chemical composition of P(VDF-DB) is VDF / DB=86:14, add a solvent to fully dissolve. Then add an appropriate amount of 3-mercapto-1-propanesulfonate sodium and an appropriate amount of deionized water. After the sodium mercaptosulfonate is completely dissolved, add an appropriate amount of catalyst in the reaction solution, whe...

Embodiment 3

[0047] This embodiment includes the following steps:

[0048] Step 1: Add the raw material P(VDF-CTFE) into the reaction bottle, and add the solvent at the same time. After fully dissolving, add a sufficient amount of catalyst triethylamine, and stir the reaction at 55°C-65°C for 24 hours. The resulting polymer solution P(VDF-DB) was precipitated with deionized water, while excess triethylamine was removed with hydrochloric acid. The precipitated polymer is soaked in methanol, and vacuum-dried to a constant weight at a temperature not higher than 50°C.

[0049] Step two:

[0050] Add the polymer P(VDF-DB) obtained in step 1 into the reaction flask, the chemical composition of P(VDF-DB) is VDF / DB=86:14, add a solvent to fully dissolve. Then add an appropriate amount of 3-mercapto-1-propanesulfonate sodium and an appropriate amount of deionized water. After the sodium mercaptosulfonate is completely dissolved, add an appropriate amount of catalyst in the reaction solution, whe...

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Abstract

The invention provides a method for preparing a P(VDF-DB)-g-S-C3H6-SO3H proton exchange membrane material. The method comprises the following steps: firstly, dissolving P(VDF-CTFE) and a catalyst intoa certain solvent; stirring and reacting for a certain time under a certain temperature condition; separating out a polymer P(VDF-DB) from de-ionized water; then, dissolving the P(VDF-DB), sodium thiosulfate and a catalyst into a certain solvent at the same time; after stirring and reacting for a certain time under a certain temperature condition, separating out a polymer in chloroform; decompressing and filtering to obtain a yellow polymer; sufficiently immersing the obtained yellow polymer by utilizing a hydrochloric acid solution (with the pH (Potential of Hydrogen) of 3); then decompressing and filtering and repeatedly immersing by utilizing methanol to remove unreacted organic matters and byproducts thereof; dissolving a washed product into acetone and sufficiently dissolving; then carrying out precipitation by utilizing n-hexane, and decompressing and filtering; finally, drying in vacuum until the weight is constant. The method provided by the invention has the advantages of simple technology, moderate conditions and easiness for obtaining the high-purity target product, and has a good industrial application prospect.

Description

technical field [0001] The present invention relates to a new method for preparing fluorine-containing polymer-based proton exchange membrane materials, in particular to a method for preparing P(VDF-DB)-g-S-C from P(VDF-CTFE) through elimination and addition reactions 3 h 6 -SO 3 H proton exchange membrane material method. Background technique [0002] The proton exchange membrane is the core part of the proton exchange membrane fuel cell, and they play the role of isolating the reactants at the two poles and providing sub-channels. Proton exchange membrane materials can be mainly divided into fluorine-free proton exchange membrane materials and fluorine-containing proton exchange membrane materials. Fluorine-free proton exchange membrane material with methylene (-CH 2 -) or benzene rings to form the main chain, which is then prepared by sulfonation. The most representative of fluorine-containing proton exchange membrane materials is DuPont's Nafion membrane product. N...

Claims

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Application Information

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IPC IPC(8): C08F214/22C08F8/00C08F8/36C08F8/26C08J5/22H01M8/1072
CPCY02E60/50Y02P70/50
Inventor 张志成牛之静李欣慰谭少博
Owner XI AN JIAOTONG UNIV
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