A kind of preparation method of composite proton exchange membrane

A proton exchange membrane and solution technology, which is applied in the field of composite proton exchange membrane preparation, can solve the problems affecting the proton conductivity of composite membranes, graphene oxide is easy to agglomerate, and the water content of the membrane is reduced, so as to achieve low methanol methanol permeability and easy Obtaining the effect of reducing the permeability of methanol

Inactive Publication Date: 2016-02-17
XIAMEN UNIV
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  • Claims
  • Application Information

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Problems solved by technology

Lin's research group (Journal of Power Sources, 2013, 237, 187-194) filtered the graphene oxide nanosheet solution on a cellulose acetate membrane. After drying, the graphene oxide was bonded to the Nafion membrane by hot pressing. Graphene oxide sheets are rich in hydroxyl and epoxy groups, graphene oxide is well compatible with Nafion membranes, and can release a large amount of H due to the presence of carboxyl groups. + , the composite membrane has a high ion exchange capacity, but the hot pressing method greatly reduces the water content of the membrane, which seriously affects the proton conductivity of the composite membrane
Chen's research group (The Journal of Physical Chemistry C, 2013, 115, 20774-20781) made a hybrid membrane by doping sulfonated graphene oxide in Nafion solution, and achieved a high proton conductivity, but because the modification method is only ordinary Physical blending, and graphene oxide is easy to agglomerate and difficult to disperse uniformly, so there are problems of heterogeneous hybrid film and phase separation

Method used

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  • A kind of preparation method of composite proton exchange membrane
  • A kind of preparation method of composite proton exchange membrane
  • A kind of preparation method of composite proton exchange membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Firstly, graphene oxide is prepared. Add 2g of graphite powder, 1g of sodium nitrate, and 46mL of concentrated sulfuric acid into a 500mL round-bottomed flask, place it in an ice bath to 0°C and keep stirring for 1 hour, remove the ice bath, then slowly add 6g of potassium permanganate while vigorously stirring, and control the temperature to a low temperature Keep at 20°C and 35°C for 1h, then add 92mL of deionized water dropwise, keep stirring at 95°C for 2h, then add 280mL of deionized water, and 40mL of 30% hydrogen peroxide solution to neutralize potassium permanganate, Centrifuge and wash the obtained product at a speed of 6000rpm, wash once with 5% dilute hydrochloric acid, wash three times with water, and finally dry the product under vacuum at 70°C for 24 hours, weigh the quality of the product obtained, and disperse the product in deionized water to obtain 2.8wt % graphene oxide aqueous solution, and ultrasonic 4h, obtain graphene oxide nanosheet solution.

...

Embodiment 2

[0037] The preparation of graphene oxide and The recasting of the 117 film was the same as in Example 1. When preparing the composite film, first prepare the assembly solution, take 525 μL of 2.8wt% graphene oxide nanosheet solution and 70 mL deionized water, and prepare a 1 mg / 5mL graphene oxide nanosheet solution, which is dispersed evenly by ultrasonic; 0.3516 g of p-diphenylamine The hydrochloride was added to 70 mL of deionized water to prepare a 0.5 wt % p-diphenylamine solution. will be preprocessed The 117 membrane is alternately placed in p-diphenylamine solution and 1mg / 5mL graphene oxide nanosheet solution for self-assembly process, each soaking in diphenylamine solution and 1mg / 5mL graphene oxide nanosheet solution is one assembly, continuous Complete 30 assemblies. The assembly time of the 117 membrane in each assembly solution should be more than 1.5h to ensure that the graphene oxide nanosheets and p-diphenylamine can be stably assembled on the membrane surf...

Embodiment 3

[0039] The preparation of graphene oxide and The recasting of the 117 film was the same as in Example 1. When preparing the composite film, first prepare the assembly solution, take 525 μL of 2.8wt% graphene oxide nanosheet solution and 70 mL deionized water, and prepare a 1 mg / 5mL graphene oxide nanosheet solution, which is dispersed evenly by ultrasonic; 0.3516 g of p-diphenylamine The hydrochloride was added to 70 mL of deionized water to prepare a 0.5 wt % p-diphenylamine solution. will be preprocessed The 117 membrane is alternately placed in p-diphenylamine solution and 1mg / 5mL graphene oxide nanosheet solution for self-assembly process, each soaking in diphenylamine solution and 1mg / 5mL graphene oxide nanosheet solution is one assembly, continuous Complete 50 assemblies. The assembly time of the 117 membrane in each assembly solution should be more than 1.5h to ensure that the graphene oxide nanosheets and p-diphenylamine can be stably assembled on the membrane su...

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Abstract

The invention discloses a preparation method of a composite proton exchange membrane, belonging to direct methanol fuel cells. Ultrasonic stripping of graphite oxide to obtain an aqueous solution of graphene oxide nanosheets; recast the Nafion solution into a film with a film thickness of 25-35 μm, and then pretreat the recast film; use the Nafion film as the base film, and p-phenylenediamine hydrochloride as Adhesive, adopting the method of layer-by-layer assembly, assembling graphene oxide on the surface of Nafion membrane to prepare a composite proton exchange membrane, and post-processing it. By assembling graphene oxide nanosheets on the Nafion membrane, the methanol permeability of the composite proton exchange membrane is greatly reduced, and its selectivity is increased to 5 times that before assembly. The Nafion base film obtained by recasting can be made very thin, reducing the amount of Nafion solution used, and because graphene oxide is easy to obtain, low cost, simple process, strong operability, and will not affect the microstructure and mechanical strength of the film. Obvious impact, no pollution to the environment.

Description

technical field [0001] The invention belongs to a direct methanol fuel cell, and in particular relates to a preparation method of a composite proton exchange membrane. Background technique [0002] Direct methanol fuel cells have the advantages of simple structure, low operating temperature and pressure, high efficiency, high energy density, environmental friendliness, convenient fuel storage, transportation and replenishment, and modularization of the device. It has a great competitive advantage and is one of the high-tech development priorities of governments. The proton exchange membrane is the core component of the membrane electrode device in the single cell of the direct methanol fuel cell. The Nafion perfluorosulfonic acid proton exchange membrane produced by DuPont of the United States is currently the most widely used fuel cell electrolyte membrane. Since the Nafion membrane has good chemical, mechanical and thermal stability, and the Nafion membrane is + High pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M2/16
CPCH01M8/0228Y02E60/50
Inventor 刘庆林王丽莎
Owner XIAMEN UNIV
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