The graphite intercalation compound with easy low temperature exfoliated and high exfoliated volume was prepared by chemical oxidation method using natural graphite flakes, C2H5COOH, FeCl3 and CrO3 as raw materials, according to the mass ratio of 1:2.8:0.3:0.2. The expansion volume of graSubscript textphite intercalation compounds was 320 mL•g-1 at 300°C and achieved biggest 580 mL•g-1 at 700°C. The composition, structure and properties of the graphite intercalation compound were characterized and analyzed by SEM, FTIR, XRD, TG, DSC, VSM techniques. Results showed that the intercalant of graphite sandwich were C2H5COO- and FeCl3.