A kind of preparation method of sulfonated polyimide proton conductive membrane containing branched structure

A technology of sulfonated polyimide membrane and sulfonated polyimide, which is applied to structural parts, circuits, electrical components, etc., can solve the problems of shortening the service life of batteries, poor anti-oxidation ability of separators, and decreasing battery capacity, etc. To achieve the effect of improving anti-oxidation, improving anti-oxidative ability and easy operation

Active Publication Date: 2017-12-19
SOUTHWEAT UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, similar to most non-fluorine polymer proton-conducting membranes, the separator has poor oxidation resistance and is easily damaged by VO in the battery. 2 + Oxidation of the solution leads to microscopic defects in the diaphragm, which causes the cross-mixing of the positive and negative electrodes to cause a decrease in battery capacity, thereby greatly shortening the service life of the battery

Method used

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  • A kind of preparation method of sulfonated polyimide proton conductive membrane containing branched structure
  • A kind of preparation method of sulfonated polyimide proton conductive membrane containing branched structure

Examples

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Effect test

Embodiment 1

[0024] in N 2 Under protection, add 2.0mmol BDSA, 50mL m-cresol, 5.0mmol triethylamine into a 250mL three-neck flask, stir continuously at room temperature until BDSA is completely dissolved, then add 1.0mmol ODA and 3.3mmol TAPOB into the container until completely dissolved; Dissolve 8.0mmol NTDA and 1.2g benzoic acid in 20ml m-cresol, place in a constant pressure dropping funnel and add slowly dropwise, and raise the temperature to 50°C for 15 hours, put the reaction solution in a clean glass The film is cast on the board, and then dried at a temperature of 60-150°C (for thermal imidization), and the branched sulfonated polyimide film of the triethylamine salt type is obtained;

[0025] The branched sulfonated polyimide membrane of the prepared triethylamine salt type was placed in acetone and soaked for 10 hours to remove excess solvent and non-participating reactants, and then soaked in 1.0mol / L sulfuric acid solution for 20 hours to make It is completely protonated, and...

Embodiment 2

[0029] in N 2 Under protection, add 3.0mmol BDSA, 60mL m-cresol, 5.0mmol triethylamine into a 250mL three-neck flask, stir continuously at room temperature until BDSA is completely dissolved, then add 1.0mmol ODA and 2.67mmol TAPOB into the container until completely dissolved; Dissolve 8.0mmol NTDA and 1.2g of benzoic acid in 30ml of m-cresol, and place in a constant pressure dropping funnel to slowly add dropwise, and raise the temperature to 50°C for 20 hours, and put the reaction solution in a clean glass The film is cast on the board, and then dried at a temperature of 60-150 ° C (for thermal imidization), that is, a triethylamine salt-type branched sulfonated polyimide film is obtained;

[0030] The branched sulfonated polyimide membrane of the prepared triethylamine salt type was placed in acetone and soaked for 24 hours to remove excess solvent and non-participating reactants, and then soaked in 1.0mol / L sulfuric acid solution for 24 hours to make It is completely pro...

Embodiment 3

[0034] in N 2 Under protection, add 4.0mmol BDSA, 70mL m-cresol, 5.0mmol triethylamine into a 250mL three-neck flask, stir continuously at room temperature until BDSA is completely dissolved, then add 2.0mmol ODA and 1.33mmol TAPOB into the container until completely dissolved; Dissolve 8.0mmol NTDA and 1.8g of benzoic acid in 30ml of m-cresol, and place it in a constant pressure dropping funnel and add it slowly, and raise the temperature to 50°C for 20 hours. Put the reaction solution on a clean glass The film is cast on the board, and then dried at a temperature of 60-150°C (for thermal imidization), and the branched sulfonated polyimide film of the triethylamine salt type is obtained;

[0035] The branched sulfonated polyimide membrane of the prepared triethylamine salt type was placed in acetone and soaked for 30 hours to remove excess solvent and non-participating reactants, and then soaked in 2.0mol / L sulfuric acid solution for 12 hours to make It is completely protona...

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Abstract

The invention discloses a preparation method of a sulfonated polyimide proton conductive membrane containing a branched structure. Ethylamine was put into the reactor, stirred at room temperature until the solid was dissolved, 1,3,5-tris(4-aminophenoxy)benzene and 4,4'-diaminodiphenyl ether were added and stirred until dissolved, and 1,4,5,8-naphthalene tetracarboxylic dianhydride and benzoic acid were dissolved in m-cresol and placed in a constant pressure dropping funnel, added dropwise to the reactor, stirred and heated to 40-100°C, reacted for 15- 24 hours; pour the reacted material onto a glass plate to form a film, then dry it at 60-150°C for 10-30 hours, then dry, soak and wash to obtain a sulfonated polyimide with a branched structure Proton-conducting membrane; the proton-conducting membrane is suitable for all-vanadium redox flow batteries and fuel cells, and has good performance.

Description

technical field [0001] The invention belongs to the preparation of a proton conductive membrane, and relates to a preparation method of a sulfonated polyimide proton conductive membrane containing a branched structure, in particular to a method containing 1,3,5-tris(4-aminophenoxy) The preparation method of the branched sulfonated polyimide proton conduction membrane of benzene (abbreviation TAPOB); Used as a battery separator in hydrogen-oxygen fuel cells, direct methanol fuel cells, etc. Background technique [0002] With the continuous growth of the global population and the depletion of resources, energy shortage has become one of the main problems facing the world at present, and the development of new energy sources that can replace petroleum products has become an important goal of today's society. All-vanadium redox flow battery (VRFB for short) is a new type of green flow battery, which was first proposed by Skyllas-Kazacos et al. in 1985; the redox pair of VRFB is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10C08J5/22C08J7/14H01M2/16H01M50/403H01M50/411H01M50/423H01M50/489
CPCY02E60/10
Inventor 张亚萍张帅黄小东张红平张永德罗学刚
Owner SOUTHWEAT UNIV OF SCI & TECH
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