Abstract: With the rapid development of lead and zinc melting technology, the wastewater composition of this smelting industry is more complex, in which efficient and green treatment technology, particularly for COD （Chemical Oxygen Demand） discharge of enterprises in China, is urgently necessary. For the current demand of the lead and zinc smelting wastewater, a novel catalytic advanced oxidation technology （KYCAOP） is applied, where its treatment effect and best working condition are also compared with the Fenton oxidation and NaClO oxidation process in detail. The results show that for the same batch of smelting wastewater （raw water COD 151 mg/L）, the removal rates of Fenton oxidation and NaClO oxidation are only 47.2% and 22.1%, while the KYCAOP is more than 75%. Besides, the oxidation rate of KYCAOP is efficient, and the COD concentration can be stabilized below 40 mg/L after 20 min of reaction, which also demonstrates the great potential of KYCAOP in lead and zinc smelting wastewater advanced treatment of COD.