The development of a catalyst with high catalytic activity was one of the most important issues for the heterogeneous Fenton-like process. In this study, nanocomposites of Fe3O4 anchored onto reduced graphene oxide (RGO) were prepared by a moderate alkaline-thermal precipitation method and developed as highly efficient heterogeneous Fenton-like catalysts. The characterization results indicated that Fe3O4 nanoparticles (NPs) were tightly anchored onto few-layer RGO sheets via a strong interaction. Contrast experiments showed that Fe3O4/RGO nanocomposites had much better Fenton-like catalytic activity than Fe3O4 NPs. The process optimization of methyl orange (MO) discoloration in Fe3O4/RGO-H2O2 system was accomplished by central composite design under response surface methodology. A second-order polynomial model was established to predict the optimal values of MO discoloration and its significance was evaluated by analysis of variance. Three-dimensional response surfaces for the interaction between two variables were constructed. Based on the model prediction, the optimum conditions for MO discoloration in Fe3O4/RGO-H2O2 system were 2.9 for solution pH, 16.5 mM H2O2 concentration, 2.5 g/L catalyst dosage and 33.5 min of reaction time, with the maximum predicted value for MO discoloration ratio of 99.98%.

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