Abstract: Jiangxi Sanhe Gold Co.，Ltd. used the pyrometallurgical smelting process to recover gold and silver from aqua regia residue，which had problems such as low recovery rate and large loss. Through systematic process technology analysis and experimental research，the combined process of wet reduction of ammonia water and hydrazine hydrate + pyrometallurgical smelting was determined，and the optimum process parameters in the wet stage were determined. Leaching time was 0.5 h，20% concentration of am‐ monia water dosage was 4 mL/g，liquid-solid ratio was 5 mL/g. Under this optimized condition，industrial practice was carried out. The results show that the combined process can significantly improve the recovery effect of silver. The direct recovery rate of silver is 22.26 percentage points higher than that of the original single fire process，and the comprehensive recovery rate is as high as 98.58%. At the same time，the puri‐ ty of gold products has been improved，and energy consumption and environmental pollution have been ef‐ fectively reduced. This process provides a technical solution for the efficient and clean recovery of gold and silver in aqua regia residue.

Key words: aqua regia slag, ammonia leaching, hydrazine hydrate reduction, silver recovery, pyromet‐ allurgical smelting