A medium-high temperature proton conduction material with nitrogen-containing microporous structure and preparation method thereof
A technology of microporous structure and proton conduction, applied in fuel cells, electrochemical generators, electrical components, etc., can solve the problems of reduced proton conductivity, high production cost, complex preparation process, etc., achieve good stability, improve proton The effect of conductivity
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[0029] The present invention also provides a method for preparing a medium-high temperature proton conduction material with a nitrogen-containing microporous structure, comprising the following steps:
[0030] Step 1: Put 2,4,6-triaminopyrimidine and 2,4,6-trihydroxy-1,3,5-benzenetricarbaldehyde into a reaction vessel, add reaction solvent and catalyst, and heat at 100-130°C React for 5 to 6 days to obtain a mixed solution;
[0031] Step 2: Rinse the mixed solution obtained in Step 1 with DMF and methanol solution to remove soluble organic matter, then use methanol to Soxhlet extract the product for 1-2 days, and dry it in a vacuum dryer at 60-100°C for 12 hours to obtain A powder material with a nitrogen-containing microporous structure.
[0032] Step 3: Soak the powder material obtained in Step 2 in concentrated phosphoric acid for 3 to 5 days, then further filter to obtain a solid dispersion loaded with phosphoric acid, and dry the solid dispersion in a vacuum dryer at 100...
Embodiment 1
[0040] Step 1: Add 1mmol monomer 2,4,6-triaminopyrimidine and 1mmol 2,4,6-trihydroxy-1,3,5-benzenetricarbaldehyde (TFP) into the reaction kettle, then add 10mL of 1,4-dioxane solvent, after stirring evenly, add 4mL of 6mol / L acetic acid as a catalyst, and react at 100°C for 6 days to obtain a mixed solution;
[0041] Step 2: Wash the mixed solution obtained in Step 1 with N,N-dimethylformamide (DMF) solution and methanol solution respectively, and extract the filtered powder with methanol for 2 days, and dry the product in vacuum at 100°C for 12 Hours, a powder material with a nitrogen-containing microporous structure.
[0042] Step 3: Soak the powder material obtained in Step 2 in concentrated phosphoric acid for 5 days, then further filter to obtain a solid dispersion loaded with phosphoric acid, and dry the solid dispersion in a vacuum dryer at 150°C for 12 hours to obtain a compound containing Medium and high temperature proton conduction material with nitrogen microporou...
Embodiment 2
[0049] Step 1: Add 1mmol monomer 2,4,6-triaminopyrimidine and 1mmol 2,4,6-trihydroxy-1,3,5-benzenetricarbaldehyde (TFP) into the reaction kettle, then add 10mL of 1,3,5-trimethylbenzene solvent, after stirring evenly, add 4mL of 6mol / L acetic acid as a catalyst, react at 130°C for 5 days, and obtain a mixed solution;
[0050] Step 2: Wash the mixed solution obtained in Step 1 with N,N-dimethylformamide (DMF) solution and methanol solution respectively, and extract the filtered powder with methanol for 1 day, and dry the product in vacuum at 60°C for 12 Hours, a powder material with a nitrogen-containing microporous structure.
[0051] Step 3: Soak the powder material obtained in Step 2 in concentrated phosphoric acid for 4 days, then further filter to obtain a solid dispersion loaded with phosphoric acid, and dry the solid dispersion in a vacuum dryer at 100°C for 12 hours to obtain a compound containing Medium and high temperature proton conduction material with nitrogen mic...
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