A Fe2O3 modified ZSM-5 hybrid was synthesized by solid phase exchange method in this work. The prepared Fe-ZSM-5 material was characterized by XRD and SEM and was used as a heterogeneous Fenton catalyst in oxidation of methylene blue. The influences of different parameters such as the initial pH value, the amount of catalyst, amount of H2O2, contact time and reaction temperature on the removal rate of methylene blue were evaluated. Results showed that under the optimum conditions of catalyst dosage of 1.1 g/L, initial pH value of 3.0, reaction temperature of 30°Cand H2O2 30 mmol/L, 98.2% of decolorization rate could be achieved in 60 minutes. This work provides a promising catalyst for the decolorization of methylene blue in aqueous solution.