Polybenzimidazole with sulfonated side chain and preparation method thereof
A polybenzimidazole and benzimidazole technology, which is applied in the parts, electrical components, circuits and other directions of fuel cells, can solve the problems of low proton conductivity, complex reaction process, and difficulty in quantitative execution.
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Embodiment 1
[0043] Embodiment 1: the synthesis of dibenzimidazole monomer
[0044] Take the synthesis of a dibenzimidazole monomer as an example: 1.0 moles of 3,3'-benzidine (purity 97%), 2.0 moles of 4-phenoxybenzoyl chloride (purity 97%) and 0.5 liter of N-methylpyrrolidone into a 1.0 liter reaction flask with nitrogen gas, mechanically stirred at 25°C for 12 hours, then heated to 180°C for 4 hours, cooled and poured into dilute NaOH aqueous solution, filtered, and water and ethanol repeated washing, vacuum drying to obtain dibenzimidazole monomer (yield 90%) can be directly used in the next step of polymerization. In the infrared spectrum at 1625cm -1 (C=N, moderately strong) the characteristic absorption peak of imidazole appears, and the reaction formula is as follows:
[0045]
Embodiment 2
[0047] In turn, 1.00 moles of 4,4'-diphenyl ether dicarboxylic acid, 0.99 moles of the dibenzimidazole monomer synthesized in Example 1, and 0.01 moles of 2,2'-bis(3-sulfonated propoxy)bis Disodium benzene, and 4 liters of Eaton's reagent were added to a nitrogen-filled reaction bottle, stirred and reacted at 80°C for 48 hours, and the reaction solution was poured into a large amount of deionized water while it was hot to obtain a polymer precipitate, filtered and washed repeatedly with deionized water until the filtrate is neutral, the obtained polymer is soaked in 0.1mol / L dilute NaOH solution at room temperature for 24 hours, then washed repeatedly with deionized water until the washing solution is neutral, and vacuum dried to obtain Na + Polymers with side chains containing sulfonic acid groups in the form of polymers. In the infrared spectrum at 1646cm -1 The characteristic absorption peak of carbonyl group appears on the left and right and the absorption peak of carboxy...
Embodiment 3
[0052] 1.00 mole of 4,4'-diphenyl ether dicarboxylic acid, 0.50 mole of dibenzimidazole monomer synthesized in Example 1, 0.50 mole of 2,2'-bis(3-sulfonated propoxy)bis Disodium benzene, prepared according to the method of Example 2, and 4 liters of Eaton's reagent were added to a nitrogen-filled reaction bottle, stirred and reacted at 100°C for 24 hours, and the reaction solution was poured into a large amount of deionized water while it was hot to obtain a polymer precipitate, filtered And wash repeatedly with deionized water until the filtrate is neutral, soak the obtained polymer with 0.1mol / L dilute NaOH solution at room temperature for 24 hours, then wash repeatedly with deionized water until the washing liquid is neutral, and vacuum dry to obtain Na + Polymers with side chains containing sulfonic acid groups in the form of polymers. In the infrared spectrum at 1646cm -1 The characteristic absorption peak of carbonyl group appears on the left and right and the absorptio...
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