Abstract: The effects of liquid-solid ratio, reaction temperature, reaction time, concentration of NaCl and concentration of sulfuric acid on the leaching rates of Pb, Sb and Bi were investigated by using Pb leached by NaCl, Sb, and Bi by sulfuric acid while NaCl leached from copper anode slime flotation tailings. The experimental results show that the leaching rates of Pb, Sb and Bi are 72.2 %, 7.83 % and 10.77 %, respectively, when the liquid-solid ratio is 5:1, the reaction temperature is 80 ℃, the reaction time is 2 h, and the concentration of NaCl is 6 mol/L. The leaching rates of Sb and Bi are 74.97 % and 84.27 %, respectively, when the liquid-solid ratio is 5:1, the reaction temperature is 60 ℃, the reaction time is 2 h, the concentration of sulfuric acid is 3 mol/L. The hydrolysis solution can be recycled after hydrolysis recovery of Sb and Bi.