Abstract: The mass concentration of (ferrous)ferric cyanide complex and copper cyanide complex is 1 500 mg/L and 510 mg/L respectively in the cyanide-containing wastewater of a gold smelting enterprise.The previous treatment process costs much and the copper cyanide complex and (ferrous)ferric cyanide complex can not be effectively separated.The experiment uses ferrous salt precipitation-acidification-hydrogen peroxide oxidation joint treatment process to treat the wastewater and the experimental conditions are optimized.Besides effective removal of cyanide,the joint process realized efficient separation of (ferrous)ferric cyanide complex and copper cyanide complex,and the valuable metal copper can be recovered in form of precipitation.The total cyanide mass concentration in the treated wastewater is below 50 mg/L,cupric ion mass concentration is below 50 mg/L,which reaches the standards of process recycling.