Abstract: Electro-Fenton process with activated carbon fiber as the cathode and Ti/SnO₂-Sb₂O₃ as the anode was used in the treatment of acetophenone wastewater. Effects of Fe²⁺ concentration and electric current density on acetophenone degradation were investigated. It was indicated that the phenyl in acetophenone molecular could be destroyed by electro-Fenton process and chemical oxygen demand (COD_Cr) of the wastewater decreased significantly. Compared with traditional two-dimensional electrode process in which no Fe²⁺ was added, the pollutant removal efficiency and current efficiency by electro-Fenton process were both higher. Current density has significant influences on the pollutant removal. Higher current density raised pollutant removal efficiency while lowering current efficiency. Under the conditions of electric current density 10.0 mA/cm², Fe²⁺ 0.1 mmol/L and initial pH 4.0, the removal efficiencies of COD_Cr and acetophenone at 180 min were 58.96% and above 90%, respectively.