Abstract: In a gold smelting enterprise， the mass concentrations of ferrocyanide and copper cyanide complexes in cyanide-containing wastewater were about 1500 mg/L and 510 mg/L， respectively. The original treatment process had high cost and could not effectively separate copper cyanide complexes from ferrocyanide. The combined process of ferrous salt precipitation-acidification-hydrogen peroxide oxidation was used to treat the wastewater， and the experimental conditions were optimized. The combined process effectively removed cyanide while achieving efficient separation of ferrocyanide and copper cyanide complexes， and valuable metal copper was recovered in the form of precipitate. After treatment， the mass concentration of total cyanide in the wastewater was lower than 50 mg/L， and the mass concentration of copper ion was lower than 50 mg/L， meeting the requirements of process reuse standards.