Preparation method of fuel cell proton membrane material solid superacid/nitrogen-heterocyclic graphene oxide/2,5-polybenzimidazole
A solid superacid and fuel cell technology, which is applied in fuel cells, electrochemical generators, circuits, etc., can solve the problems of low energy conversion rate of proton exchange membranes and difficulty in forming continuous proton conduction, and achieve excellent battery performance, proton Excellent electrical conductivity and the effect of improving proton conductivity
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Embodiment 1
[0043] Embodiment 1: Preparation of 2,5-polybenzimidazole (ABPBI)
[0044] (1) Purification method of monomer 3,4-diaminobenzoic acid: Add a certain amount of 3,4-diaminobenzoic acid into water at 70°C, slowly add hydrazine hydrate until it is completely dissolved, and then add an appropriate amount to the mixture Activated carbon was kept at 70°C for 30 minutes, filtered, cooled, and recrystallized with acetic acid.
[0045] (2) Preparation steps of 2,5-polybenzimidazole (ABPBI):
[0046]
[0047] The purified 3,4-diaminobenzoic acid (4.0g, 26.4mmol) was added to the reaction solvent of 40ml polyphosphoric acid (PPA) (containing 6g P 2 o 5 ). Slowly raise the temperature to 220°C under the protection of nitrogen, change the polymerization reaction time, and stop the polymerization reaction after mechanical stirring for 20 minutes, 30 minutes, and 40 minutes respectively, and pour the hot solution into deionized water to obtain fine fibers. The fibers were collected and...
Embodiment 2
[0048] Embodiment 2: the preparation of graphite oxide
[0049] Slowly add 1g of expanded graphite into a 23ml large beaker filled with concentrated sulfuric acid under stirring, keep the temperature at (0±1)°C, then slowly and continuously add the mixture of 1g of sodium nitrate and 3.0g of potassium permanganate, while stirring Maintain at (0±1)°C for 2 hours. In a constant temperature water bath at (35±3)°C, keep stirring for 30 minutes, slowly add deionized water to raise the temperature to 98°C, and maintain this temperature for 15 minutes. Dilute with warm water, pour into hydrogen peroxide (30%), filter while hot, fully wash the filter cake with 5% HCl until there is no sulfate ion in the filtrate (detected by barium chloride solution). Dry in a vacuum oven at 50°C and store in a sealed container until use.
Embodiment 3
[0050] Embodiment 3: the preparation of functionalized graphene oxide
[0051] The synthetic method of functionalized graphene oxide (NGO) such as Figure 9 shown
[0052] (1) Disperse 1 g of graphite oxide prepared in Example 2 above in 10 ml of sodium dodecylbenzene sulfonate solution, and ultrasonically disperse for 1 hour to obtain graphene oxide wrapped in a surfactant.
[0053] (2) Adjust the above (1) step solution to alkaline, that is, adjust the pH to 10 with 1M NaOH, add 5ml of 60% hydrazine hydrate and stir at 50°C for 24 hours, then remove the aggregated product with a funnel to obtain surface active The chemically modified (reduced) product wrapped in the agent was centrifuged, washed 5 times, and dried to collect the product, and then the product was formulated into a 1 mg / ml aqueous solution for use.
[0054] (3) Preparation of diazonium salt: R-NH containing triazole group (R) in ice water bath (0°C) 2 Compounds and NaNO 2 and HBF 4 The diazonium tetrafluo...
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