In order to recover value elements copper, bismuth and antimony in lead electrolysis refining anodic slime bearing high antimony and lower silver comprehensive, the process route is as follows: from the solution leached drydistillation residue in AC process by water Cu, Bi and Cu were cemented with iron powders in two steps; copper was leached with a sulphuric acid solution from the residue, and bismuth was leached with dilution hydrochloric acid from the leached copper residue. The cemented ratio of Cu, Bi and Sb is 99.75%, 96.74% and 99.45% respectively, in the cemented residues containing Cu 62.26% and Bi 20.79%. The separation of copper from antimony and bismuth was realized by leaching copper with sulphate acid solution. Copper was used for production of copper suphate containing CuSO4·5H2O 93.74%～96.12% and Fe 1.13%～1.47% with recovery ratio of 93.33%. Direct recovery ratio of bismuth is 90.87% into a concentrate containing Bi of 69.70% and sum ratio is 94.73%. In addition, an antimony residue containing Sb of 36.21% was produced with recovery ratio of 94.06%.