Preparation method of three-dimensional graphene co-doped with iron and nitrogen
A co-doping and graphene technology, applied in graphene, chemical instruments and methods, structural parts, etc., can solve the problems of metals being easily removed by acid, low catalytic performance, and insufficient durability
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Embodiment 1
[0014][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 w...
Embodiment 2
[0015] [Example 2] Synthesis of mPBI by solid-phase method: DABz (4g, 18.7 mmol) and isophthalic acid (3.1g, 18.7 mmol) were mixed in a mortar, thoroughly ground and mixed, and transferred to a stirrer with nitrogen protection. in the three-neck flask. Nitrogen was passed 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 mPBI, and the molecular weight of mPBI was measured with an Ubbelohde viscometer.
[0016] The preparation method of ABPBI is similar to that of mPBI, except that 3,4-diaminobenzoic acid (DABA) is used instead of DABz and isophthalic acid. ABPBI can be obtained using only one raw material. Other reaction conditions and operation steps are with embodiment...
Embodiment 3
[0017] [Example 3] MgO with a particle diameter of 30 nm is used as a template, the mass ratio of ferric acetate and PBI for iron salt is 1:2, and mPBI is used for PBI, and the mass ratio of mPBI and MgO template is 1:1 as an example: In a 250mL beaker, add 1g of mPBI (viscosity-average molecular weight: 30,000 to 50,000) and 20mL DMAc, heat and stir to dissolve, add 0.5 g of iron acetate in 20mL DMAc solution under stirring, and keep warm at 80°C to 100°C , stirring and reacting for 5-8 hours, slowly adding 1 g of nanometer MgO particles with a particle size of 30 nm, and stirring for 4-6 hours to make them uniformly dispersed. The obtained viscous liquid was heated and concentrated to nearly dryness under stirring, and dried in a vacuum oven at 100°C. The solid was ground in a mortar, transferred to a porcelain boat, and kept in an electric furnace at 900°C under the protection of argon. Pyrolyze for 2-3 hours, wait for the furnace temperature to drop to room temperature, ta...
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