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Aiming at the removal of refractory organic pollutants in aqueous solution, self-assembled nano-Fe₃C embedded in reduced graphene oxide (nano-Fe₃C@RGO) aerogel was prepared by hydrothermal synthesis and high temperature treatment, and characterized by SEM, HRTEM, pore size distribution, XRD, XPS and FTIR. The results showed that the aerogel was porous, and most of the Fe₃C particles were less than 100 nm in size. They were evenly dispersed and embedded in the RGO aerogel. Furthermore, the mapping images confirmed that the elements of carbon, nitrogen and iron were homogeneously distributed. Moreover, the specific surface area of the aerogel was up to 324.770 m²/g and most of the pore sizes were between 5 and 10 nm. The formation of nano-Fe₃C was identified by XRD pattern and HRTEM. Analysis of an XPS spectrum indicates that the nano-Fe₃C was embedded in the graphene layer. The aerogel contained a large number of functional groups, including –NH₂, –NH and –C=O, etc., which greatly strengthened the adsorption of organics. Finally, the Fenton-like catalytic degradation properties of the self-assembled nano-Fe₃C@RGO aerogel were investigated by testing the removal of methyl orange from the aqueous solution. The results showed that the value of C_t/C₀ decreased to 0.050 after 240 min, suggesting a high degradation rate was obtained. Meanwhile, the chemical reaction was verified in accordance with the first-order kinetic model, and the higher temperature was beneficial to the catalytic degradation. At the same time, methyl orange was degraded into small molecules by the hydroxyl and superoxide radicals generated during the reactions. Therefore, the self-assembled nano-Fe₃C@RGO aerogel, as a novel Fenton-like catalyst, introduces a new approach in the field of treatment of refractory organic wastewater. Full article