Preparation of Fe-Co-N three-element co-doping three-dimensional graphene with catalytic synergistic effect
A synergistic and co-doping technology, applied in physical/chemical process catalysts, electrical components, chemical instruments and methods, etc., can solve the problems of easy removal of metals by acid, poor durability, and low catalytic performance.
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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 ...
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 size of 30nm is used as a template, both iron salt and cobalt salt use acetate, and the molar ratio is 1:1; the mass ratio between the two salts and PBI is 1:2 after mixing, and mPBI is used for PBI , taking the mass ratio of mPBI to MgO template as 1:1 as an example: in a 250mL beaker, add 1g of mPBI (viscosity average molecular weight 20,000 to 30,000) and 20mL DMAc, heat and stir to dissolve, then add 0.5 g of a mixture of cobalt acetate and iron acetate (the two salts are mixed at a molar ratio of 1:1) in 20 mL of DMAc solution, kept at 80 ° C to 100 ° C, stirred for 5 to 8 hours, slowly added 1 g of 30 nm particle size Nano MgO particles, stirred for 4~6 hours to make it evenly dispersed. The obtained viscous liquid was heated and concentrated to nearly dryness under stirring, and dried in a vacuum oven at 120°C. The solid was ground in a mortar, transferred to a porcelain boat, and kept in an electric furnace at 900°C under the prot...
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