Polypyrron with sulfated side chain and preparation method of polypyrron
A technology of sulfonation and polypyridine, which is applied in electrochemical generators, fuel cell parts, fuel cells, etc., can solve problems such as difficulty in synthesizing sulfonated aromatic tetraamine monomers
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Embodiment 1
[0050] Embodiment 1: the synthesis of dipyrrolene monomer
[0051] The dipyrrolene monomer is obtained from the condensation reaction between the dianhydride compound and the aryl diamine compound. Take the synthesis of a dipyrrone monomer as an example: 1.0 moles of 1,8-naphthalene dicarboxylic anhydride (97% purity), 2.2 moles of 3,4-diaminodiphenyl ether (97% purity) ), 0.05 moles of zinc acetate and 0.5 liters of N-methylpyrrolidone were added to a 1.0-liter reaction bottle with nitrogen gas, mechanically stirred at 180 ° C for 4 hours, cooled, poured into water, filtered, washed with water and ethanol repeatedly, vacuum After drying, the dipyrrolene monomer (yield: 95%) was obtained, which may be a mixture of cis-trans isomers but does not affect the polymerization, and can be directly used in the next step of polymerization. In the infrared spectrum at 1698cm -1 (C=O, strong) left and right and 1617cm -1 、1548cm -1 (=C=N, weaker) the characteristic absorption peak of...
Embodiment 2
[0054] Sequentially add 1.00 moles of 4,4'-diphenyl ether dicarboxylic acid, 0.99 moles of the dipyrone monomer synthesized in Example 1, and 0.01 moles of 2,2'-bis(3-sulfonated propoxy)biphenyl Add disodium and 4 liters of Eaton's reagent into a nitrogen-filled reaction bottle, stir and react at 80°C for 48 hours, pour the reaction solution into a large amount of deionized water while hot to obtain a polymer precipitate, filter and wash repeatedly with deionized water until the filtrate is Neutral, soak the obtained polymer with 0.1mol / L dilute hydrochloric acid at room temperature for 24 hours, then wash repeatedly with deionized water until the washing solution is neutral, and vacuum dry to obtain H + Polymers with side chains containing sulfonic acid groups in the form of polymers. In the infrared spectrum at 1698cm -1 (C=O, strong) left and right and 1617cm -1 、1548cm -1 (=C=N, weaker) appeared the characteristic absorption peak of pyrolone and 1646cm -1 Carbonyl abso...
Embodiment 3
[0059] Sequentially add 1.00 moles of 4,4'-diphenyl ether dicarboxylic acid, 0.50 moles of the dipyrrolene monomer synthesized in Example 1, and 0.50 moles of 2,2'-bis(3-sulfonated propoxy)biphenyl Disodium (prepared according to the method in Example 2) and 4 liters of Eaton reagent were added to a nitrogen-filled reaction bottle, stirred and reacted at 100°C for 24 hours, the reaction solution was poured into a large amount of deionized water while it was hot to obtain a polymer precipitate, filtered and used Wash with deionized water repeatedly until the filtrate is neutral, soak the obtained polymer with 0.1mol / L dilute hydrochloric acid at room temperature for 24 hours, then wash repeatedly with deionized water until the washing liquid is neutral, and vacuum dry to obtain H + Polymers with side chains containing sulfonic acid groups in the form of polymers. In the infrared spectrum at 1698cm -1 (C=O, strong) left and right and 1617cm -1 、1548cm -1 (=C=N, weaker) appear...
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