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A classic carbon material—expanded graphite (EG), was prepared and proposed for a new application as catalysts for activating peroxydisulfate (PDS). EG samples prepared at different expansion temperatures were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and other methods. It was observed that there existed a remarkable synergistic effect in the EG/PDS combined system to degrade Acid Red 97 (AR97). Unlike other carbon material catalysts, sp2 carbon structure may be the main active site in the catalytic reaction. The EG sample treated at 600 °C demonstrated the best catalytic activity for the activation of PDS. Degradation efficiency of AR97 increased with raising PDS dosage and EG loadings. The pH of aqueous solution played an important role in degradation and adsorption, and near-neutrality was the optimal pH in this research. It was assumed that the radical pathway played a dominant role in AR97 degradation and that oxidation of AR97 occurred in the pores and interface layer on the external surface of EG by SO4·− and ·OH, generated on or near the surface of EG. The radical oxidation mechanism was further confirmed by electron paramagnetic resonance spectroscopy. The EG sample could be regenerated by annealing, and the catalytic ability was almost fully recovered.

Preparation and Catalytic Performance of Expanded Graphite for Oxidation of Organic Pollutant