The invention relates to a preparation method of nano-graphite carbon powder. The method comprises the steps of: (1) preparing expansible graphite by a chemical oxidation intercalation process; (2) preparing expanded graphite by a microwave process; (3) pressing the expanded graphite into a expanded graphite sheet, putting it into a microporous filter membrane sieving assembly, conducting pressing and sealing, then placing the assembly at the anode and cathode of an electrolytic bath, taking a chlorate solution as an electrolyte solution, carrying out ultrasonic electrolysis at a temperature below 60DEG C, controlling the electrolytic current at 5-18A / cm<2>, the voltage at 6-20V, the ultrasonic oscillation power at 200-600W, and the frequency at 20-40kHz, inverting the anode and the cathode at an interval of 8-15min, completing electrolysis when the concentration of sol in the electrolytic bath is 2-5%, thus obtaining nano-graphite carbon sol; and (4) adding ammonium sulphate into the nano-graphite carbon sol till the mass concentration of ammonium sulfate reaches 5-8%, stirring them uniformly, then performing freeze drying, thus obtaining the nano-graphite carbon powder. The method has the advantages of mild reaction condition and high speed, thus being suitable for industrialized mass production.