A kind of preparation method of graphene-based carbon nanospheres
A nano-carbon sphere and graphene-based technology, applied in the field of nano-materials, can solve the problems of complex preparation process, unfavorable promotion, high reaction temperature, etc., and achieve the effect of simple preparation process, rich pore structure and uniform distribution
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[0071]The specific embodiment part of the present invention provides a kind of preparation method of graphene-based nano-carbon sphere, and described preparation method comprises the following steps:
[0072] (1) prepare graphene oxide dispersion liquid;
[0073] (2) in the graphene oxide dispersion that step (1) obtains, add H 2 o 2 React with a reducing agent under stirring, and separate the solid and liquid after the reaction is completed to obtain a carbon sphere dispersion;
[0074] (3) purifying and separating the carbon sphere dispersion obtained in step (2), and vacuum freeze-drying the solid obtained after the separation to obtain graphene-based nano carbon spheres.
Embodiment 1
[0077] (1) Graphene oxide was prepared by the Hummers method, and the graphene oxide was ultrasonically dispersed in water for 1 h with a power of 50 W to obtain a graphene oxide dispersion with a concentration of 1.5 mg / mL;
[0078] (2) the hydroxylamine solution is added dropwise in the graphene oxide dispersion liquid of step (1) gained, the mass ratio of hydroxylamine and graphene oxide is 3:1, then add H 2 o 2 solution, where H 2 o 2 10:1 mass ratio to hydroxylamine, using CH 3 COONH 4 The pH of the solution was adjusted to 7, and the reaction was carried out with stirring at 25°C for 24 hours. After the reaction was completed, it was filtered with a polytetrafluoroethylene filter membrane to obtain a carbon sphere dispersion;
[0079] (3) Using a dialysis bag with a molecular weight of 3500Da, the carbon sphere dispersion obtained in step (2) was dialyzed for 48 hours, and then vacuum freeze-dried at -50°C for 48 hours to obtain graphene-based carbon nanospheres.
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Embodiment 2
[0082] (1) The graphene oxide was prepared by the Hummers method, and the graphene oxide was ultrasonically dispersed in water for 1.5h, and the power was 60W to obtain a graphene oxide dispersion with a concentration of 2mg / mL;
[0083] (2) N-methylhydroxylamine solution is added dropwise in the graphene oxide dispersion liquid of step (1) gained, the mass ratio of N-methylhydroxylamine and graphene oxide is 2:1, then add H 2 o 2 solution, where H 2 o 2 The mass ratio with N-methylhydroxylamine is 10:1, the pH of the solution is adjusted to 7 by using NaOH solution, and the reaction is carried out with stirring at 25° C. for 36 hours. After the reaction is completed, filter with a polytetrafluoroethylene membrane to obtain a carbon sphere dispersion;
[0084] (3) Using a dialysis bag with a molecular weight of 3000Da, the carbon sphere dispersion obtained in step (2) was dialyzed for 72 hours, and then vacuum freeze-dried at -50°C for 48 hours to obtain graphene-based carbo...
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