In the process of cyanidation of gold concentrate, such minerals as copper and zinc partially enter into the liquid, resulting in a gradual increase in its mass fraction. In order to purify the cyanide-containing liquid and realize the efficient recovery of copper and zinc, it is determined that the pH values of zinc precipitation and copper precipitation are 5.99 and 3.69 respectively based on the analysis of complexation stability constants of related substances. Through the test of different pH values, sodium sulfide dosage and reaction time of cyanide-containing liquids, the yield grades of zinc and copper reach 42.97% and 58.33%, respectively, and the precipitation rates of zinc and copper reach 94.13% and 98.30%, respectively. The R&D of this process achieves the purpose on fractional reduction of purifying the copper and zinc complexation ions in the barren liquor, effectively reducing the mass fraction of copper and zinc ions, realizing the comprehensive utilization of copper and zinc resource recovery in cyanide-containing wastewater, while the treated barren liquor is conducive to improving the leaching rate of gold and silver in the gold concentrate during the leaching process.