Preparation method of fluorine-containing branched sulfonated polyimide proton conducting membrane

A technology of sulfonated polyimide and proton conductive membrane, which is applied in circuits, electrical components, battery pack components, etc., can solve the problems of low resistance to vanadium, reduction, and weak oxidation resistance, and achieve strong oxidation resistance , high proton conductivity, and the effect of reducing vanadium permeability

Inactive Publication Date: 2017-11-24
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention aims to overcome the shortcomings of the existing non-fluorine polymer SPI membranes, which have weak oxidation resistance and low vanadium resistance performance, and use fluorine-containing "Y" type triamine monomer as one of the raw materials to synthesize fluorine-containing branched sulfonate fluorine-containing branched sulfonated polyimide proton-conducting membrane, and the prepared f

Method used

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  • Preparation method of fluorine-containing branched sulfonated polyimide proton conducting membrane

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Embodiment 1

[0028] A preparation method for a fluorine-containing branched sulfonated polyimide proton conductive membrane, the steps of which are:

[0029] in N 2 Under protection, add 8.0mmol NTDA, 20mL m-cresol, and 9.8mmol benzoic acid into a 250mL three-neck flask, and stir continuously at room temperature until NTDA and benzoic acid are completely dissolved; dissolve 2.0mmol BDSA in a 50mL m- Add 5.0mmol triethylamine dropwise to cresol, wait until BDSA is completely dissolved, then add 1.0mmol ODA and 3.3mmol TFAPOB into the beaker to dissolve completely, and place it in a constant pressure dropping funnel and slowly drop it into a three-necked flask. And the temperature was raised to 60°C for 15 hours to obtain a film solution containing fluorine-branched SPI. The reaction solution was cast on a clean glass plate to form a film, and then dried at a temperature of 60-150°C for 20 hours (preferably a gradient , that is, the temperature is gradually increased in a gradient to dry), ...

Embodiment 2

[0034] A preparation method for a fluorine-containing branched sulfonated polyimide proton conductive membrane, the steps of which are:

[0035] in N 2 Under protection, add 8.0mmol NTDA, 30mL m-cresol, and 9.8mmol benzoic acid into a 250mL three-neck flask, and stir continuously at room temperature until NTDA and benzoic acid are completely dissolved; into cresol, and dropwise added 5.0mmol triethylamine, until BDSA was completely dissolved, then added 1.0mmol ODA and 2.67mmol TFAPOB into the beaker to dissolve completely, and placed in a constant pressure dropping funnel and slowly added dropwise into a three-neck flask, And the temperature was raised to 50°C for 20h to obtain a film solution containing fluorine-branched SPI. The reaction solution was cast on a clean glass plate to form a film, and then dried at a temperature of 60-150°C for 23h (preferably a gradient , that is, the temperature is gradually increased in a gradient to dry), that is, a triethylamine salt-type...

Embodiment 3

[0040] A preparation method for a fluorine-containing branched sulfonated polyimide proton conductive membrane, the steps of which are:

[0041] in N 2 Under protection, add 8.0mmol NTDA, 30mL m-cresol, and 14.7mmol benzoic acid into a 250mL three-neck flask, and stir continuously at room temperature until NTDA and benzoic acid are completely dissolved; dissolve 4.0mmol BDSA in a 70mL m- Add 5.0mmol triethylamine dropwise to cresol, wait until BDSA is completely dissolved, then add 2.0mmol ODA and 1.33mmol TFAPOB into the beaker to dissolve completely, and place it in a constant pressure dropping funnel and slowly drop it into a three-necked flask. And the temperature was raised to 50°C for 20h to obtain a film solution containing fluorine-branched SPI. The reaction solution was cast on a clean glass plate to form a film, and then dried at a temperature of 60-150°C for 25h (preferably a gradient , that is, the temperature is gradually increased in a gradient to dry), that is,...

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Abstract

The invention discloses a preparation method of a fluorine-containing branched sulfonated polyimide proton conducting membrane. The preparation method is characterized by comprising the following steps: under protection of nitrogen gas, adding m-cresol, 1,4,5,8-naphthalene tetracarboxylic dianhydride and benzoic acid into a reactor, and stirring until solid substances are dissolved; adding m-cresol, 2,2'-disulfonic acid benzidine and triethylamine into a container, stirring until the solid substances are dissolved, then adding 1,3,5-tri(2-trifluoromethyl-4-aminophenoxy)benzene, 4,4'-diaminodiphenyl ether to stir to dissolve to obtain a mixture; putting the mixture in a constant-pressure dropping device, and dropwise adding the mixture into a reactor, stirring and heating for 15-24 hours at temperature of 40-100 DEG C; then casting a reacted material into a membrane, and drying the membrane; then soaking and washing to prepare the fluorine-containing branched sulfonated polyimide proton conducting membrane. The prepared fluorine-containing branched sulfonated polyimide proton conducting membrane is good in performance, and is suitable for the fields of all-vanadium redox flow cells, hydrogen oxygen fuel cells, direct methanol fuel cells and the like.

Description

technical field [0001] The invention belongs to the preparation of battery separators, and relates to a preparation method of a fluorine-containing branched sulfonated polyimide proton conductive membrane. The prepared fluorine-containing branched sulfonated polyimide proton conductive membrane is suitable for the fields of all-vanadium redox flow battery, hydrogen-oxygen fuel cell, direct methanol fuel cell and the like. Background technique [0002] With the rapid development of society and economy, people's demand for energy is increasing, and the shortage of traditional fossil energy has become an important problem that all countries in the world must face. my country will accelerate the development of renewable energy such as solar energy, tidal energy, and wind energy as a basic national policy. However, these new renewable energy sources will be affected by factors such as time, temperature, season, day and night, making the power generation process discontinuous and...

Claims

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Application Information

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IPC IPC(8): C08J5/22C08J7/02C08G73/10H01M2/16C08L79/08H01M50/409
CPCC08G73/1071C08J5/2256C08J7/02C08J2379/08H01M50/409Y02E60/10
Inventor 张亚萍杨攀蒲阳周雨芹轩森森
Owner SOUTHWEAT UNIV OF SCI & TECH
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