Preparation method of polybenzoxazine reinforced three-dimensional graphene foam
A technology of graphene foam and polybenzoxazine, which is applied in the direction of graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of restricting widespread use, structural damage, high temperature, etc., and achieve a simple and easy preparation method, high Mass preparation, effect of large specific surface area
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[0031] As a preparation method of polybenzoxazine reinforced three-dimensional graphene foam, the method steps are as follows:
[0032] (1) Graphene oxide is ultrasonically dispersed in deionized water to obtain an aqueous graphene oxide solution;
[0033] (2) Then dissolve a certain amount of benzoxazine monomer in an organic solvent, slowly add it dropwise to the graphene oxide dispersion in step (1), ultrasonicate and stir for a period of time (the time of stirring ultrasonically is 0.5-8h). After the solution is fully mixed evenly, it is transferred to a high-pressure reactor, and the hydrothermal reaction is carried out at a certain temperature;
[0034] (3) After reacting for a period of time, the (2) reactor is cooled to room temperature, the hydrogel after the reaction is taken out, and the unreacted benzoxazine monomer is removed by repeated washing with deionized water and an organic solvent;
[0035] (4) The hydrogel in (3) is freeze-dried to obtain a polybenzoxazi...
Embodiment 1
[0040] First, the improved Hummers method was used to prepare graphene oxide, and a 4 mg / ml graphene oxide aqueous solution (50ml) was prepared by ultrasonic and mechanical stirring, followed by 0.4% (mass concentration) of 3,4-dihydro-1 3. The acetone solution (2.5ml) of benzoxazine was slowly added dropwise (0.5ml / min) into the graphene oxide dispersion, ultrasonicated and stirred for 6 hours, then transferred to the reaction kettle. Reacting the reactor with the mixed solution at 100° C. for 6 hours to obtain a polybenzoxazine-reinforced graphene hydrogel. After the hydrogel was washed and freeze-dried for 48 hours, a polybenzoxazine-enhanced three-dimensional graphene foam was obtained. Then put the polybenzoxazine-enhanced three-dimensional graphene foam into a quartz tube, heat up to 800°C under the protection of 200 sccm argon, and anneal for 3 hours. After the furnace temperature is cooled to room temperature, the three-dimensional graphene airgel is obtained. Its den...
Embodiment 2
[0042] First, the improved Hummers method was used to prepare graphene oxide, and a 4mg / ml graphene oxide aqueous solution (50ml) was prepared by means of ultrasonic and mechanical stirring, followed by 2% 3,4-dihydro-1,3 benzo The acetone solution / ml (2.5ml) of oxazine and the toluene solution (2.5ml) of 2% diphenylmethane diamine type benzoxazine are slowly added dropwise (0.5ml / min) in the graphene oxide dispersion liquid successively , Ultrasonic and stirred for 6h, then transferred to the reaction kettle. React the reaction kettle with the mixed solution at 160° C. for 6 hours to obtain a thermosetting polybenzoxazine-reinforced graphene hydrogel. After the hydrogel was washed and freeze-dried for 48 hours, a polybenzoxazine-enhanced three-dimensional graphene foam was obtained. Then put the polybenzoxazine-enhanced three-dimensional graphene foam into a quartz tube, heat up to 800°C under the protection of 200 sccm argon, and anneal for 3 hours. After the furnace temper...
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