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Method for preparing high-temperature proton exchange membrane

A technology of proton exchange membrane and high temperature, which is applied in the field of preparation of high temperature proton exchange membrane, can solve the problems of affecting proton conductivity, affecting proton conductivity, proton conductivity reduction, etc., and achieves excellent high temperature proton conductivity and oxidation resistance, Continuous and long-distance proton conduction, the effect of enhancing the ability of proton conduction

Active Publication Date: 2014-05-07
UNIV OF SCI & TECH OF CHINA
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Problems solved by technology

At present, the research on high-temperature proton exchange membranes in the world is still in its infancy, and the research basically only focuses on the selection of membrane materials.
At present, despite the low price of hydrocarbon membranes, its application and development are restricted due to poor thermal and chemical stability; at the same time, the performance of new hydrocarbon polymers still has a long way to go. , so that the application of high-temperature proton exchange membrane fuel cells is greatly limited
For example, the Hayami research group (Journal of the American Chemical Society (2013, 135, 8097-8100)) made graphene oxide into nanosheets, using a large number of epoxy groups on its surface, and the formation of hydroxyl and carboxyl groups with water Hydrogen bonds greatly improve its high temperature water retention, making it have better proton conduction ability at high temperature and 100% humidity. However, the solid powder characteristics and intercrystalline boundaries of graphene oxide itself affect its long-distance and long-lasting sexual proton conductivity
Hwang research group (Advanced Energy Materials (2011,1,1220-1224)) doped graphene oxide in sulfonated polyimide, due to the sulfonic acid groups of polyimide and the water retention of graphene oxide It has high proton conductivity at 90°C and 60% humidity, but when it is greater than 100°C, the cross-linking of sulfonic acid groups and the reduction of humidity will cause its proton conductivity to decrease. Separation, graphene oxide may be detached from the membrane, which will also affect its proton conductivity
Scott's research group (Journal of Materials Chemistry (2011, 21, 11359-11364)) respectively doped graphene oxide and sulfonated graphene oxide into polybenzimidazole to form a high-temperature anhydrous proton exchange membrane, and explored The structural mechanism of polybenzimidazole interpenetrating between graphene oxide sheets is understood, and its conductance at high temperature can reach 52mS / cm, but because it is only an ordinary physical mixture, there is still a phase separation problem, and then this film There is a tendency to decrease the conductivity at temperatures above 150°C, reflecting the possibility of graphene oxide detachment from the film layer and loss of water retention of graphene oxide

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  • Method for preparing high-temperature proton exchange membrane
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  • Method for preparing high-temperature proton exchange membrane

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Embodiment 1

[0034] This embodiment prepares the high temperature proton exchange membrane according to the following steps:

[0035] (1) Preparation of graphene oxide-metal organic framework: Ultrasonic dispersion of 0.03 g graphene oxide in 10 mL of water-ethanol mixture (volume ratio of water and ethanol is 1:1) to obtain mixture A, and then metal organic framework The precursor synthesis of the framework (0.1g basic zinc carbonate, 0.1g oxalic acid and 0.4g 3-amino-1,2,4-triazole) was ultrasonically dispersed in the obtained mixture A, and reacted for 72 hours at 180°C to obtain the product Wash with water and ethanol three times respectively, and then dry at 60° C. (dry for 4 hours) to obtain a brown-black graphene oxide-metal-organic framework coexistence body.

[0036] (2) Preparation of N-methylpyrrolidone solution of sulfonylchlorinated polyphenylene ether: Dissolve 0.2g of sulfonated polyphenylene ether in 1mL (0.9445g) of N,N-dimethylformamide, and slowly Add 0.5mL (0.838g) of ...

Embodiment 2

[0043] This embodiment prepares the high temperature proton exchange membrane according to the following steps:

[0044] (1) Preparation of graphene oxide-metal organic framework: Ultrasonic dispersion of 0.06 g graphene oxide in 10 mL of water-ethanol mixture (volume ratio of water and ethanol is 1:1) to obtain mixture A, and then metal organic framework The precursor synthesis of the framework (0.1g basic zinc carbonate, 0.1g oxalic acid and 0.4g 3-amino-1,2,4-triazole) was ultrasonically dispersed in the obtained mixture A, and reacted for 72 hours at 180°C to obtain the product Wash with water and ethanol three times respectively, and dry at 60°C (dry for 4 hours) to obtain a brown-black graphene oxide-metal organic framework coexistence body.

[0045] (2) Preparation of N-methylpyrrolidone solution of sulfonylchlorinated polyphenylene ether: Dissolve 0.2g of sulfonated polyphenylene ether in 1mL (0.9445g) of N,N-dimethylformamide, and slowly Add 0.5mL (0.838g) of thionyl...

Embodiment 3

[0052] (1) Preparation of graphene oxide-metal organic framework: Ultrasonic dispersion of 0.09 g graphene oxide in 10 mL of water-ethanol mixture (volume ratio of water and ethanol is 1:1) to obtain mixture A, and then metal organic framework The precursor synthesis of the framework (0.1g basic zinc carbonate, 0.1g oxalic acid and 0.4g 3-amino-1,2,4-triazole) was ultrasonically dispersed in the obtained mixture A, and reacted for 72 hours at 180°C to obtain the product Wash with water and ethanol three times respectively, and then dry at 60° C. (dry for 4 hours) to obtain a brown-black graphene oxide-metal-organic framework coexistence body.

[0053] (2) Preparation of N-methylpyrrolidone solution of sulfonylchlorinated polyphenylene ether: Dissolve 0.2g of sulfonated polyphenylene ether in 1mL (0.9445g) of N,N-dimethylformamide, and slowly Add 0.5mL (0.838g) of thionyl chloride dropwise, a white precipitate is formed, wash and filter with water, and dry at 60°C (dry for 2 ho...

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Abstract

The invention discloses a method for preparing a high-temperature proton exchange membrane. The method is characterized by comprising the following steps: introducing a precursor composition with a metal organic frame into oxidized graphene to form a coexisting body of the oxidized graphene and the metal organic frame, subsequently adding the coexisting body together with a sodium hydroxide solution into an N-methyl pyrrolidone solution of sulfonyl chlorination polyphenyl ether to perform Hinsberg reaction to obtain polymer membrane casting liquid with the coexisting body, coating and drying so as to obtain the high-temperature proton exchange membrane. According to the method, the metal organic frame is introduced into the oxidized graphene by using a hydrothermal method to form the coexisting body, and is further prepared into the high-temperature proton exchange membrane together with sulfonated polyphenyl ether in a chemical bond mode, the membrane is good in mechanical strength, thermal stability and excellent high-temperature proton conductivity and oxidative resistance, and can be applied to high-temperature proton exchange membrane fuel batteries.

Description

technical field [0001] The invention belongs to the technical field of high-temperature proton exchange membranes, and in particular relates to a preparation method of a novel graphene oxide-metal organic framework-based high-temperature proton exchange membrane. Background technique [0002] Increasing the working temperature of the fuel cell is one of the effective measures to solve the complex water heat management of the battery and the poisoning of the catalyst; at the same time, it can also improve the kinetics of the oxygen reduction reaction at the anode and cathode of the battery, especially the cathode, thereby improving the working efficiency of the battery. Therefore, high-temperature proton exchange membrane fuel cell technology has become the main direction of fuel cell development today. [0003] As one of the key materials of proton exchange membrane fuel cell, the working temperature of proton exchange membrane determines the working temperature of fuel cell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M8/12H01M8/1226
CPCC08J5/2256C08J2371/12H01M8/1041H01M8/1051H01M2008/1095Y02E60/50Y02P70/50
Inventor 徐铜文伍斌
Owner UNIV OF SCI & TECH OF CHINA
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