In order to recover gold and silver from anode slimes containing Cu, Ni, Sn, and Zn, an integrated hydrometallurgical process consisting of leaching, solvent extraction, and cementation was developed. All the metals together with 10% of Ag(I) were dissolved by the mixture of HCl and H2O2 at the optimum conditions. Separation of Au (III) together with Sn (II) was performed by Cyanex 272 from the leaching solution with two-stage counter current extraction. Stripping of Au (III) and Sn (II) from the loaded organic phase was sequentially carried out by NH4Cl and NaOH. Cu (II) in the raffinate after Au (III) extraction was separated by LIX 63 with three-stage counter current extraction. Pure Cu (II) solution was recovered from the loaded LIX 63 by stripping with dilute HCl solution. Ag powders with extra high purity were obtained by cementation with copper sheet from the raffinate after Cu (II) separation. Au (III) (99.3%) and 96.8% of Sn (II) were recovered by extraction, and purity of Au (III) and Sn (II) stripping solutions was found to be 99.99%. Au powders with extra high purity were directly synthesized by adding ascorbic acid solution into the NH4Cl stripping solution.