Zinc leaching residue is a good source of zinc and has a great potential to be utilized. However, it is very difficult to recover lead, zinc and silver from the residue by traditional technologies. In this study, a new technology based on conversions of PbSO4 and ZnSO4 in the residue to their respective sulfides by reduction roasting with coal powder followed by a flotation treatment was developed. The effects of roasting temperature, coal dosage, reaction time and pyrite dosage were investigated at a laboratory scale. The results showed that the conversion extent of PbSO4 and ZnSO4 under the optimal experimental conditions was 71.89 and 69.76%, respectively. A flotation concentrate containing 39.13% Zn, 6.93% Pb and 973.54 g/Mg Ag was obtained from the treated material, and the recovery of Zn, Pb and Ag was 48.38, 68.23 and 77.41%, respectively. The tailing containing ZnFe2O4 or Fe3O4 could be either stockpiled or further disposed.