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Preparation method of self-crosslinking sulfonated polyimide film

A sulfonated polyimide membrane and self-crosslinking technology, which can be used in energy storage, electrochemical generators, bulk chemical production, etc., can solve the problem of unfavorable sulfonated polyimide membrane proton conduction and membrane chemical stability It is difficult to significantly improve or affect polymer film formation and physical and chemical properties, so as to improve proton transfer ability and solve the effect of weak chemical stability

Active Publication Date: 2020-07-10
SOUTHWEAT UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ionic crosslinking will consume part of the sulfonic acid groups used for proton transfer, which is not conducive to the proton conduction of sulfonated polyimide membranes; at the same time, the hydrogen bonds formed by ionic crosslinking are weak, which will improve the chemical stability of the membrane. has certain limitations
Covalent cross-linking requires the use of external cross-linking agents and special cross-linking sites. The amount of cross-linking agents is generally limited, so it is difficult to significantly improve the chemical stability of the separator; at the same time, the covalent cross-linking process and conditions need to be precise. Control, once the cross-linking agent is excessive, it will directly affect the film-forming and physical and chemical properties of the polymer

Method used

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  • Preparation method of self-crosslinking sulfonated polyimide film
  • Preparation method of self-crosslinking sulfonated polyimide film
  • Preparation method of self-crosslinking sulfonated polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A preparation method of self-crosslinking sulfonated polyimide membrane, comprising the following steps:

[0036] Step 1. Under the protection of nitrogen, add 8mmol of 1,4,5,8-naphthalene tetracarboxylic dianhydride, 8mmol of benzoic acid, and 40mL of m-cresol into a 250mL three-necked flask in turn, and stir until the solid is completely dissolved; then, add 1.3 mmol 4,4'-diaminodiphenyl ether, 1.3mmol 4,4',4",4"'(5,5'-benzimidazole-2,2')-1,3(phenylene)- Add tetraoxytetraphenylamine, 4mmol 2,2'-disulfonic benzidine, 4mmol triethylamine, and 40mL m-cresol into a 100mL beaker, stir until the solids are completely dissolved; then place the liquid in the beaker under constant pressure drop Slowly add it dropwise into the three-necked flask, and stir the material in the reactor while adding dropwise, and the dropwise time is 10min; the temperature is raised to 60°C, and stirred for 4h; then, the reaction solution is poured on a glass plate, Cast a film, and dry in an oven...

Embodiment 2

[0044] A preparation method of self-crosslinking sulfonated polyimide membrane, comprising the following steps:

[0045] Step 1. Under the protection of nitrogen, add 8mmol of 1,4,5,8-naphthalene tetracarboxylic dianhydride, 8mmol of benzoic acid, and 40mL of m-cresol into a 250mL three-necked flask in sequence, and stir until the solid is completely dissolved; then, add 0.8 mmol 4,4'-diaminodiphenyl ether, 1.6mmol 4,4',4",4"'(5,5'-benzimidazole-2,2')-1,3(phenylene)- Add tetraoxytetraphenylamine, 4mmol 2,2'-disulfonic benzidine, 4mmol triethylamine, and 40mL m-cresol into a 100mL beaker, stir until the solids are completely dissolved; then place the liquid in the beaker under constant pressure drop Slowly add it dropwise into the three-necked flask, and stir the material in the reactor while adding dropwise, and the dropwise time is 10min; the temperature is raised to 60°C, and stirred for 4h; then, the reaction solution is poured on a glass plate, Cast into a film, and dry i...

Embodiment 3

[0053] A preparation method of self-crosslinking sulfonated polyimide membrane, comprising the following steps:

[0054]Step 1. Under the protection of nitrogen, add 8mmol of 1,4,5,8-naphthalene tetracarboxylic dianhydride, 8mmol of benzoic acid, and 40mL of m-cresol into a 250mL three-necked flask in turn, and stir until the solid is completely dissolved; then, add 2.0 mmol 4,4'-diaminodiphenyl ether, 1.0mmol 4,4',4",4"'(5,5'-benzimidazole-2,2')-1,3(phenylene)- Add tetraoxytetraphenylamine, 4mmol 2,2'-disulfonic benzidine, 4mmol triethylamine, and 40mL m-cresol into a 100mL beaker, stir until the solids are completely dissolved; then place the liquid in the beaker under constant pressure drop Slowly add it dropwise into the three-necked flask, and stir the material in the reactor while adding dropwise, and the dropwise time is 10min; the temperature is raised to 60°C, and stirred for 4h; then, the reaction solution is poured on a glass plate, Cast into a film, and dry in an ...

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Abstract

The invention discloses a preparation method of a self-crosslinking sulfonated polyimide film, which comprises the following steps: under the protection of nitrogen, adding m-cresol I, 1,4,5,8-naphthalenetetracarboxylic dianhydride and benzoic acid into a reactor, and stirring at room temperature until dissolution; adding 4,4'-diaminodiphenyl ether, 4,4',4'',4'''(5,5'-benzimidazole-2,2')-1,3-(phenylene)-tetraoxy tetraphenylamine, 2,2'-benzidinedisulfonic acid, triethylamine and m-cresol II into a vessel, stirring at room temperature until dissolution, then adding the materials in the vessel into a constant-pressure dropping funnel, dropwise adding into the reactor, stirring for reaction to obtain viscous fluid, pouring the viscous fluid onto a dry and clean glass plate, casting to form a film, and then drying to obtain a triethylamine salt type self-crosslinking sulfonated polyimide film; soaking the triethylamine salt type self-crosslinking sulfonated polyimide film in absolute ethylalcohol, then soaking the film in a sulfuric acid aqueous solution, and then washing the film to obtain the self-crosslinking sulfonated polyimide film. According to the invention, the problem of weakchemical stability of the sulfonated polyimide film can be solved in a targeted manner.

Description

technical field [0001] The invention belongs to the field of organic synthesis and battery diaphragm, and relates to a preparation method and application of a self-crosslinked sulfonated polyimide membrane. Background technique [0002] The shortage of traditional fossil energy (such as: coal, oil, natural gas, etc.) and the environmental problems caused by its use have become one of the main bottlenecks restricting the sustainable development of the economy and the improvement of living standards. Therefore, the utilization of new renewable energy sources (for example: solar energy, tidal energy, wind energy, etc.) has been highly valued. However, the new renewable energy power generation process is easily affected by environmental factors such as time, day and night, and seasons, and has obvious discontinuity and instability. Therefore, equipped with high-efficiency energy storage devices can effectively solve the problems of unsteady power generation of new renewable ene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08J7/02C08J7/14C08L79/08C08G73/10H01M8/0221
CPCC08J5/18C08J7/02C08J7/14C08G73/1071C08G73/1042C08G73/1085C08G73/1028H01M8/0221C08J2379/08Y02P20/54
Inventor 李劲超张亚萍胥文杰段浩龙俊刘军汪妍林罗欢
Owner SOUTHWEAT UNIV OF SCI & TECH
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