Abstract: In a certain place in Anhui polymetallic sulfide ore is high-grade sulphur associated copper、gold、silver、iron elements. Against the ore characteristics, copper -selective flotation-magnetic separation of flotation-tailing-roasting of Sulphur concentrade-cyanidation of Acid-residue is flowsheet and the final results: copper concentrate grade 20.39%, Sulphur concentrate grade 50.85%,the gold total recovery 80.81%, the silver total recovery 70.66%, iron concentrate grade 64.44%.The flowsheet is fit for the multi -metal sulfide minerals to provide a economical and reasonable,technically feasible.