Abstract: The process of recovering valuable metals of purification residue from zinc hydrometallurgy with citric acid was studied. The leaching behavior of valuable metals from purification residue was analyzed by single factor test. The effects of citric acid concentration, leaching temperature, ratio of liquid to solid, stirring speed, pH value and leaching time on the leaching rate of valuable metals were investigated. The results showed that the leaching rates of zinc, nickel and copper were 79.60%, 75.09% and 9.70%, respectively, and that of cobalt was as high as 97.64%, under the conditions of citric acid concentration 0.8 mol/L, leaching temperature 60 ℃, ratio of liquid to solid 10:1, stirring speed 200 r/min, pH1.0 and leaching time 90 min. This research provides a new way for comprehensive recovery and utilization of purification residue from zinc hydrometallurgy.