Experimental research of acidification decyanation is carried out on the cyanide residue in a gold mine,which optimizes test conditions such as concentrated sulfuric acid dosage and reaction time,and finally gives proposed process,namely the cyanide residue slurry preparation-acidification decyanation-press filter process.When the concentrated sulfuric acid dosage is 10 mL/L and the reaction time is 1.0 h,the cyanide residue after detoxification treatment can meet the requirement of tailings pond disposal standards according to HJ 943—2018 Technical Specification for Pollution Control of Cyanide Leaching Residue in Gold Industry,and the reagent cost is about 11.00 yuan/t cyanide residue.The research results can provide data reference for the industrial application of cyanide residue detoxification treatment in the gold mine.