Abstract: The sulfur concentrate of a certain high sulfur lead-zinc mine in Yunnan province contains lead and zinc, they mainly exist in galena and sphalerite. The size of sphalerite is fine, and the size of galena is finer, they are mainly composed of a large number of rich aggregate, but the dissociation degree of sphalerite is relatively better. Experimental studies were carried out, that take lime inhibit pyrite, cupric activate sphalerite, DF-341 for collector, though once-roughing twice-scavenging and fourth-cleanings after that of rough concentrate regrinding was recommend, the fineness of regrinding is -45 μm 92%, the Pb-Zn mixed concentrate was got and the sum of lead and zinc grade is 54.96%, yield is 3.16%. Based on the recommended process, a 700 t/d mill plant was built, adopting advanced and applicable equipment after optimizing the reasonable processing technology, and good benefits have been achieved.