Preparation method of three-dimensional nitrogen-doped graphene with enhanced mass transfer type multi-level channels
A nitrogen-doped graphene and channel technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as performance degradation, specific surface area reduction, and resistance increase
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Embodiment 1
[0017] [Example 1] Preparation of ABPBI (method 1, solid-phase method): Take an appropriate amount of 3,4-diaminobenzoic acid (DABA) in a mortar, grind it thoroughly and then transfer it to a three-port chamber equipped with electric stirring and inert gas protection. In the flask, pass nitrogen gas for 15 minutes to exhaust the air in the flask. N 2 Protected and stirred, heated in an oil bath at 225°C for 3h. Take it out after cooling, grind finely, N 2 Under protection, heat in an electric furnace, raise the temperature to 270-275°C, and keep it for 3 hours. After cooling to room temperature, the product was taken out and finely ground to obtain ABPBI, and the molecular weight of ABPBI was measured with an Ubbelohde viscometer.
Embodiment 2
[0018] [Example 2] Preparation of ABPBI (method 2, liquid phase method): polyphosphoric acid (PPA) (50 g) was added into a three-necked flask, stirred under nitrogen protection, and kept at 160 ° C for 1 h to remove water and air. 3,4-diaminobenzoic acid (6 g, 39.5 mmol) was added and the temperature was raised to 190 °C, controlled by N 2 The flow rate is to prevent DABA from being oxidized, and the reaction is stirred at 200°C for 3 hours. During the reaction, about 5g P 2 o 5 To absorb the water formed during the reaction. With the increase of reaction time, the polymerization system gradually became viscous. The reaction mixture was slowly transferred to deionized water, spinning to form a fibrous black solid, which was taken out and dried, crushed, and washed to remove polyphosphoric acid and unreacted raw materials in the reaction mixture. Get ABPBI products. The molecular weight of ABPBI was determined with an Ubbelohde viscometer.
Embodiment 3
[0019] [Example 3] Using nanoscale calcium carbonate particles with a particle size of 30nm as a template and mixing with ABPBI, three-dimensional porous nitrogen-doped graphene was prepared by pyrolysis. Take the mass ratio of ABPBI and nano-scale calcium carbonate template as 1:1 as an example:
[0020] In a 250mL beaker, add 1g of ABPBI (viscosity-average molecular weight 20,000 to 30,000) and 20mL of DMAc, heat and stir to dissolve, and slowly add 1g of calcium carbonate with a particle size of 30nm under stirring to disperse evenly. 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 1000°C under the protection of argon. Under pyrolysis, keep warm for 2 hours, finish heating, wait for the furnace temperature to drop to room temperature, take it out, and grind it finely to obtain a bla...
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