Preparation method of phosphotungstic acid-polyimide composite proton exchange membrane

A technology of proton exchange membrane and polyimide, which is applied in the field of preparation of phosphotungstic acid-polyimide composite proton exchange membrane, can solve the problems of heteropolyacid loss and other problems, and achieve the improvement of proton conductivity and the reduction of methanol permeability , The effect of simple preparation method

Inactive Publication Date: 2013-01-09
INNER MONGOLIA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, heteropolyacids have good water solubility. Under the conditions of medium temperature DMFC operation, heteropolyacids are easily lost with the water generated by the electrodes.

Method used

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  • Preparation method of phosphotungstic acid-polyimide composite proton exchange membrane

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Experimental program
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Effect test

Embodiment 1

[0028] 1), 4.79 grams of diphenyl ether diamine and 5.21 grams of pyromellitic dianhydride were dissolved in 90 g of dimethyl sulfoxide to form polyamic acid solution A;

[0029] 2) Solution A was stirred in a nitrogen atmosphere for 1 hour, heated to 65°C, added 2.17 g of concentrated phosphoric acid with a concentration of 85.54% by mass, 2.43 g of sodium tungstate and 8.18 g of water, and stirred for 2 hours to form a uniform solution B ;

[0030] 3) Heat the solution B to 120°C in a vacuum oil bath, continue to stir until all the water in the solution evaporates, and cool to room temperature to obtain a uniform solution C;

[0031] 4), pour solution C on a glass plate, place it flat in a drying oven, and heat it at 120°C, 150°C, 200°C, 250°C and 300°C for 12h, 1h, 1h, 1h and 1h in sequence, after cooling and falling off , that is to obtain phosphotungstic acid-polyimide composite proton exchange membrane.

[0032] When used, the membrane was soaked in deionized wate...

Embodiment 2

[0034] 1), 2.4 grams of diphenyl ether diamine and 2.6 grams of pyromellitic dianhydride were dissolved in 57.5 g of dimethyl sulfoxide to form polyamic acid solution A;

[0035] 2) Stir the solution A in a nitrogen atmosphere for 0.5h, raise the temperature to 60°C, add 1.17g concentrated phosphoric acid, 1.14g sodium tungstate and 5.23g water to the solution A, and form a uniform solution B after stirring for 3 hours;

[0036] 3) Heat the solution B in a vacuum oil bath to 110°C, continue to stir until all the water in the solution evaporates, and cool to room temperature to obtain a uniform solution C;

[0037] 4), pour solution C on a glass plate and place it flat in a drying oven, heat at 120°C, 150°C, 200°C, 250°C and 280°C for 12h, 1h, 1h, 1h and 1h in sequence, after cooling and falling off That is, the phosphotungstic acid-polyimide composite proton exchange membrane is obtained.

Embodiment 3

[0039] 1), 6.23 grams of diphenyl ether diamine and 6.77 grams of pyromellitic dianhydride were dissolved in 131.44 g of dimethyl sulfoxide to form polyamic acid solution A;

[0040] 2) Stir the solution A for 1 hour in a nitrogen atmosphere, raise the temperature to 70°C, add 3.26 g of concentrated phosphoric acid, 2.79 g of sodium tungstate and 11.95 g of water to the solution A, and stir at this temperature for 1.5 hours to form a uniform Solution B;

[0041] 3) Heat the solution B in a vacuum oil bath to 115°C, continue to stir until all the water in the solution evaporates, and cool to room temperature to obtain a uniform solution C;

[0042] 4), pour solution C on a glass plate and place it flat in a drying oven, heat at 120°C, 150°C, 200°C, 250°C and 290°C for 12h, 1h, 1h, 1h and 1h in sequence, after cooling and falling off That is, the desired phosphotungstic acid-polyimide composite proton exchange membrane is obtained.

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Abstract

The invention discloses a preparation method of a phosphotungstic acid-polyimide composite proton exchange membrane. Diphenyl ether diamine and benzenetetracarboxylic anhydride with equal molar weight are added in dimethyl sulfoxide solvent to synthesize polyamide acid solution, deionized water, sodium tungstate and concentrated phosphoric acid are then added for heating and stirring to form a solution, the solution is poured on a glass plate, the glass plate is flatly placed in an oven in a stepped temperature rise mode for imidization, and the phosphotungstic acid-polyimide composite proton exchange membrane is obtained. The preparation method is simple in method, the cost of prepared membrane is low, and the membrane is even in distribution, and conductivity and alcohol blocking performance are obviously improved. Compared with a Nafion membrane, the phosphotungstic acid-polyimide composite proton exchange membrane prepared by the method obviously improves proton conduction performance at high temperature (lower than 100 DEG C), carbinol permeability is reduced, swelling degree is reduced, cost is lowered, and the preparation method brings convenience to mass production.

Description

[0001] technical field [0002] The invention relates to a preparation method of a phosphotungstic acid-polyimide composite proton exchange membrane, belonging to the field of battery electrolyte materials. Background technique [0003] Direct methanol fuel cell (DMFC) is a proton exchange membrane fuel cell fueled by liquid methanol. Due to the advantages of cheap and easy to obtain fuel, high specific energy, convenient fuel storage and transportation, and low environmental pollution, it has gained popularity as a new type of power supply in recent years. Widespread concern. [0004] However, although the Nafion membrane used in direct methanol fuel cells has the advantages of good chemical stability, high proton conductivity, and long service life, it is not only expensive, but also has poor stability of the high-temperature proton membrane and high methanol permeability. And these two shortcomings increase with the increase of temperature, which cannot meet the requirem...

Claims

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Application Information

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IPC IPC(8): C08J5/22C08L79/08C08K3/24C08K3/32C08G73/10H01M8/10H01M8/106
CPCY02E60/522Y02E60/50Y02P70/50
Inventor 郭贵宝刘媛媛安胜利刘书题
Owner INNER MONGOLIA UNIV OF SCI & TECH
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