Highly effective Fe 3 O 4 /Mn 3 O 4 /reduced graphene oxide (rGO) hybrids were synthesized as a heterogeneous catalyst for the degradation of organic dyes in the aqueous solution using sulfate radicalbased advanced oxidation processes. The physicochemical properties of the composite were characterized 10 by several techniques, such as X-ray diffraction (XRD), Raman spectroscopy, Fourier transform infrared (FTIR), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and Brunauer-Emmelt-Teller (BET). The effects of different parameters on the catalytic activity of Fe 3 O 4 /Mn 3 O 4 /rGO, including initial Methylene Blue (MB) concentration, peroxymonosulfate (PMS) concentration, catalyst dosage, pH value, and temperature, were assessed. Typically, 98.8% removal of 50 15 mg/L of MB and 68.3% reduction of TOC could be achieved in 30 min under the conditions: temperature 25 °C, 100 mg/L of catalyst, and PMS dosage 0.3 g/L, showing a significant enhancement of the catalyst in the degradation of organic pollutants in aqueous solution Compared with Fe 3 O 4 /rGO and Mn 3 O 4 /rGO. The catalyst exhibited high stability and good reusability according to three successive repeated reactions. Based on the radical experiments, the catalytic activity of Fe 3 O 4 /Mn 3 O 4 /rGO hybrids for degradation of 20 MB is closely related with the amount of the sulfate and hydroxyl radicals generated from PMS. The excellent catalytic performance of the Fe 3 O 4 /Mn 3 O 4 /rGO is mainly attributed to the synergistic effects of Fe 3 O 4 , Mn 3 O 4 , rGO, and Oxone. 65 supporting metal and metal oxides attributed to its high electrical conductivities, unique mechanical strength, and large specific surface areas 10,11 . It has been found that graphene can This journal is © The Royal Society of Chemistry [year] conditions: catalyst = 100 mg/L, PMS dose = 0.3 g/L, initial MB concentration = 50 mg/L. pH=7.0, T = 25 °C) Fig. 6 MB degradation in the Fe3O4/Mn3O4/rGO/PMS system: the effect of initial MB concentration (a), the effect of catalyst dosage (b), the effect of PMS dosage (c), and the effect of initial pH value (d). (Except for the investigated parameter, other parameters fixed on: catalyst = 100 mg/L, Oxone dose = 0.3 g/L, initial MB concentration = 50 mg/L, pH=7.0, and T = 25 °C) 60The effect of reaction temperature on MB degradation was also investigated and the results were shown in Fig. 7. A general trend