Phosphoric acid grafted polyimide high-temperature proton exchange membrane and preparation method thereof

A proton exchange membrane and polyimide technology, which is applied in the field of phosphonic acid grafted polyimide high temperature proton exchange membrane and its preparation, can solve the problems of service temperature limitation, easy leakage of phosphonic acid, etc. leakage, good mechanical properties, good hydrolytic stability

Inactive Publication Date: 2015-04-08
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sulfonated polyimide proton exchange membrane is formed by polymerizing sulfonated diamine, non-sulfonated diamine, and diamine monomer. By controlling the ratio of sulfonated diamine and non-sulfonated diamine, the polyimide can be controlled. However, sulfonic acid cannot be ionized in the dehydration state, and the service temperature is strictly limited, so sulfonated polyimide proton exchange membranes are generally difficult to work at high temperatures
Phosphonic acid doped polyimide proton exchange membrane can operate at high temperature, but the phosphonic acid doped in the proton exchange membrane is easy to leak

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A kind of preparation method of phosphonic acid grafted polyimide high temperature proton exchange membrane, comprises the steps:

[0030] (1) Put 1mmol of 4,4'-diaminobiphenyl and 5ml of acetic acid in the reactor, stir, and slowly add 1.2mmol of liquid bromine dropwise, stir for 4h, after the reaction is completed, filter, wash with water and dry Dry to obtain brominated diamine.

[0031] (2) Dissolve the product obtained in step (1) in tetrahydrofuran at 1wt%, place it in a three-necked flask, blow nitrogen into it, cool at -78°C, slowly add an appropriate amount of n-butyllithium dropwise and stir for 30 minutes, add 2mmol of dimethyl chlorophosphate was stirred for 3 hours. After the reaction was completed, the reacted material was poured into acetone to produce a flocculent precipitate, which was filtered, washed repeatedly, and dried to obtain the product.

[0032] (3) Under the protection of nitrogen, put the product obtained in step (2), 25ml m-cresol, and 1ml...

Embodiment 2

[0037] A kind of preparation method of phosphonic acid grafted polyimide high temperature proton exchange membrane, comprises the steps:

[0038] (1) Put 1mmol of 4,4'-diaminobiphenyl and 5ml of acetic acid in the reactor, stir, and slowly add 1.2mmol of liquid bromine dropwise, stir for 4h, after the reaction is completed, filter, wash with water and dry Dry to obtain brominated diamine.

[0039] (2) Dissolve the product obtained in step (1) in tetrahydrofuran at 1wt%, place it in a three-necked flask, blow nitrogen into it, cool at -78°C, slowly add an appropriate amount of n-butyllithium dropwise and stir for 30 minutes, add 4mmol of dimethyl chlorophosphate was stirred for 3 hours. After the reaction was completed, the reacted material was poured into acetone to produce a flocculent precipitate, which was filtered, washed repeatedly, and dried to obtain the product.

[0040](3) Under the protection of nitrogen, put the product obtained in step (2), 25ml m-cresol, and 1ml ...

Embodiment 3

[0045] A kind of preparation method of phosphonic acid grafted polyimide high temperature proton exchange membrane, comprises the steps:

[0046] (1) Place 1mmol of 4,4'-diaminodiphenyl ether and 5ml of acetic acid in a reactor, stir, and slowly add 1.2mmol of liquid bromine dropwise, stir for 4h, after the reaction is completed, filter, wash with water and Dry to obtain brominated diamine.

[0047] (2) Dissolve the product obtained in step (1) in tetrahydrofuran at 1 wt%, place it in a three-necked flask, pass nitrogen gas, cool at -78°C, slowly add an appropriate amount of butyllithium and stir for 30min, add 4mmol Dimethyl chlorophosphate, and stirred for 3 hours, after the reaction, the reacted material was poured into acetone, resulting in flocculent precipitate, filtered and washed repeatedly, and dried to obtain the product.

[0048] (3) Under the protection of nitrogen, put the product obtained in step (2), 25ml m-cresol, and 1ml triethylamine into the reactor, stir a...

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Abstract

The invention belongs to the technical field of a fuel battery and particularly relates to a phosphoric acid grafted polyimide high-temperature proton exchange membrane and a preparation method thereof. The proton exchange membrane is prepared by a method comprising the following steps: firstly performing a bromination reaction on a benzene ring of a common diamine monomer to obtain bromized diamine; replacing bromine on the bromized diamine with phosphonate by using n-butyllithium and chlorophosphate so as to obtain phosphate grafted diamine; performing polycondensation reaction by using the phosphate grafted diamine, the common diamine and dianhydride to prepare the polyimide; and finally hydrolyzing the phosphonate on the polyimide by using trimethyl bromo-silicane and hydrochloric acid to prepare the phosphoric acid grafted polyimide high-temperature proton exchange membrane. The proton exchange membrane prepared by the method disclosed by the invention is excellent in proton conduction capability at a high temperature; the phosphoric acid is chemically boned in a polymer, hard to leak and good in hydrolysis resistance and stability; the phosphoric acid can also cooperate with N in the polyimide to form a continuous hydrogen bond network so as to realize water-free proton conduction.

Description

technical field [0001] The invention belongs to the technical field of fuel cells, and in particular relates to a high-temperature proton exchange membrane grafted with phosphonic acid polyimide and a preparation method thereof. Background technique [0002] Proton exchange membrane fuel cell is a new type of fuel cell, which can convert the chemical energy generated by the reaction of fuel and oxidant into electrical energy, and has the characteristics of high efficiency and environmental protection. However, at present, the operating temperature of proton exchange membrane fuel cells is low, and electrocatalysts are prone to CO poisoning, so noble metals such as Pt have to be used as electrocatalysts. Proton exchange membrane is the key material of proton exchange membrane fuel cell. The widely used nafion membrane cannot conduct proton at high temperature. Therefore, it is of far-reaching significance to synthesize a new type of proton exchange membrane that can work at h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J5/22H01M8/02H01M8/0221
CPCY02E60/50
Inventor 沈春晖李伟余剑英李慧琳尹珊珊刘超
Owner WUHAN UNIV OF TECH
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