Copper in a copper-iron polymetallic ore is mainly in the form of chalcopyrite, with a mass fraction of 0.26%. Iron is mainly in the form of pyrrhotite, magnetite and limonite, with a mass fraction of 27.88%. Arsenic is mainly in the form of toxic sand, with a mass fraction of 0.76%. Its mineral embedding has a fine particle size and a close symbiotic relationship with each other, which is a complex copper-iron polymetallic ore with high sulfur and high arsenic. Based on the nature and characteristics of the ore, a systematic beneficiation test is carried out, the separation process of "preferential copper separation-weak magnetic iron separation, iron separation, iron-sulfur separation" is formulated, and the recovery effect of copper and iron in the process of raw ore separation is effectively improved by using Z - 200 as the copper collector to strengthen the re-grinding of crude concentrate and desulfurization of iron concentrate. The closed-circuit test obtains copper concentrate with a copper grade of 25.25%, a recovery rate of 81.81% and an arsenic mass fraction of 0.16%, and an iron concentrate with an iron grade of 64.98%, a recovery rate of 33.26% and a sulfur mass fraction of 0.15%, which realizes the efficient separation and comprehensive recovery of copper, iron and sulfur minerals, and provides references for the development and utilization of similar resources.