Abstract: In order to produce crude bismuth and comprehensively recovery of valuable metals from anode slime with high silver and bismuth, The process is Two-stage leaching. The first stage is leaching of copper with sulfuric acid and the second stage is leaching of bismuth with hydrochloric acid. Studied on the relationship between the Leaching rate and the leaching temperature, time, ratio of liquid to solid (Quality), dosage of acid and oxidant.The leaching rate (Liquid) of copper is above 96 %, and The leaching rate (Slag) of bismuth and antimony are all above 99 %.The lead and silver are enriched in the second stage leaching slag, which containing Pb about 26.63 %, Ag about 36.77 %, the direct yield of Pb and Ag are 97.82 % and 98.93 % respectively.The process is cycle leaching, washing water and washing acid are returned to the next leaching, which greatly reduced the amount of wastewater, and good for environmental protection.