In this paper, it can be seen that the optimum mixture ratio of graphite to other contents (graphite: H2SO4: H2O2: HClO4) is 10(g):28(ml):1(ml):5(ml), which obtained the best expansion voluSubscript textme (191ml/g). The Fe3O4-expanded graphite composite material was prepared by FeCl3solution of ethylene glycol with heating reaction in reactor. The graphite sheets within EG were nanoscales, four iron oxide nanoparticles were dispersed between holes of expanded graphite sheets. Evidently, the graphite nanosheets wrapped in the four iron oxide particles can be observed. It is clearly that the magnetic adsorption properties of particles are strength on EG/Fe3O4. In addition, the EG/Fe3O4composite obtained by this process has a product (magnetite), which is proved of XRD characteristic peaks.