Ti/SnO2-Sb2O3/SnO2-Sb2O3-CeO2 anodes were prepared by brush coating with high temperature oxidation. The anodes were characterized by X-ray diffractometer (XRD), scanning electron microscope and cyclic voltammetry. The surface of the electrode shows more compact and exist shallower mud cracks than the others by coating with 1% Ce to the surface of Ti/SnO2-Sb2O3 electrode. The XRD patterns show that as-prepared electrodes are SnO2 and TiO2. The electrode with 1% Ce dopant shows the highest efficiency in the electrolysis of caprolactam wastewater. The oxygen evolution potential is about 1.75 V, the removal rate of chemical oxygen demand is 50%, and the biochemical oxygen demand is 353 mg/L for 5 h at a current of 0.12 A.

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