Three-dimensional nitrogen-doped graphene with hierarchical channels prepared from polybenzimidazole
A nitrogen-doped graphene and pore technology, which is applied in the manufacture of hybrid/electric double-layer capacitors, catalysts for physical/chemical processes, structural parts, etc., can solve problems such as inability to mix templates, reduced catalytic performance, and reduced active sites.
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Embodiment 1
[0017] [Example 1] Preparation of mPBI: Add polyphosphoric acid (PPA) (100 g) into a three-necked flask equipped with electric stirring and nitrogen protection, and stir at 160° C. for 1 h under nitrogen protection to remove excess water and air. DABz (4g, 18.7mmol) and isophthalic acid (3.1g, 18.7mmol) were mixed evenly, and slowly added into a three-necked flask. The nitrogen flow rate was controlled to prevent DABz from being oxidized, and at the same time, the reaction temperature was raised to 200° C., and the reaction was continued for 5-8 hours with insulation and stirring. With the increase of reaction time, the polymerization system gradually became viscous. Stop the reaction when the viscosity is appropriate, slowly transfer the reaction mixture to a large amount of deionized water, spin, wash, dry, pulverize, and wash with deionized water several times to remove polyphosphoric acid and unreacted reactants to obtain mPBI. The molecular weight of mPBI was determined ...
Embodiment 2
[0018] [Example 2] Synthesis of oPBI: Add polyphosphoric acid (PPA) (100 g) into a three-necked flask equipped with electric stirring and nitrogen protection, and stir at 160° C. for 2 hours under nitrogen protection to exclude air and moisture. DABz (4g, 18.7mmol) and 4,4'-diphenyl ether dicarboxylic acid (4.83g, 18.7mmol) were mixed evenly, and slowly added into a three-necked flask. Control the nitrogen flow rate to prevent DABz from being oxidized, and at the same time raise the reaction temperature to 200°C and continue to keep warm and stir for 5~8h. With the increase of reaction time, the polymerization system gradually became viscous. Stop the reaction when the viscosity is right, and slowly transfer the reaction mixture to a large amount of deionized water to spin, wash, dry, pulverize, and wash with deionized water several times to remove polyphosphoric acid and unreacted reactants to obtain oPBI. The molecular weight of oPBI was determined with an Ubbelohde viscome...
Embodiment 3
[0019] [Example 3] Use calcium carbonate particles with a particle size of 30nm as a template to mix with mPBI, and the mass ratio of mPBI to nanoscale calcium carbonate template is 1:1 as an example:
[0020] In a 250mL beaker, add 1g of mPBI (viscosity-average molecular weight: 30,000 to 50,000) and 20mL of DMAc, heat and stir to dissolve it, and slowly add 1g of calcium carbonate with a particle size of 30nm to disperse evenly while stirring. The obtained viscous liquid is heated and concentrated to nearly dryness under stirring, and dried in a vacuum oven at 100°C. The solid is ground in a mortar, transferred to a porcelain boat, and kept in a high-temperature electric furnace at 900°C under the protection of argon. Pyrolyze under heat, keep warm for 2-3h, wait for the furnace temperature to drop to room temperature, take it out, grind it finely to obtain a black powdery solid, transfer it to a 250mL Erlenmeyer flask, add 70mL of 3mol / L hydrochloric acid, heat, stir for 8h,...
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