A novel CuO–CeO2–Co3O4 nanocatalyst loaded on Al2O3 ceramic composite membrane (CCM-S) was synthesized through spraying-calcination method, which can be beneficial to the engineering application of scattered granular catalyst. BET and FESEM-EDX testing revealed that CCM-S possessed a porous character with high BET surface area of 22.4 m2/g and flat modified surface with extremely fine particle aggregation. The CCM-S calcined above 500 °C presented excellent anti-dissolution effect due to the formation of crystals. XPS indicated that the composite nanocatalyst possessed the variable valence states, which were conducive to exert the catalytic effect of Fenton-like reaction. Subsequently, the effects of experimental parameters including fabricate method, calcination temperature, H2O2 dosage, initial pH value, and CCM-S amount were further investigated considering the removal efficiency of Ni(II)-complex and COD after decomplexation and precipitation (pH = 10.5) treatment within 90 min. Under the optimal reaction condition, the residual Ni(II)-complex and Cu(II)-complex concentration from actual wastewater was all lower than 0.18 mg/L and 0.27 mg/L, respectively; meanwhile, the removal efficiency of COD was all higher than 50% in the mixed electroless plating effluent. Besides, the CCM-S could still maintain high catalytic activity after a six-cycle test, and the removal efficiency was slightly declined from 99.82% to 88.11%. These outcomes indicated that CCM-S/H2O2 system was provided with a potential applicability on treatment of real chelated metal wastewater.
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