Abstract: The high−sulfur complex and refractory copper−zinc polymetallic ore in Chenjiaba, Lueyang County, Shaanxi Province, has significant differences in the content of useful minerals and a close distribution relationship of useful minerals. It belongs to the refractory sulfide copper−zinc ore. It belongs to a difficult−to−select sulfide copper−zinc ore.The sequential priority flotation process of copper, zinc, and sulfur was adopted, and the effects of grinding fineness, types and dosages of reagents on the separation of copper, zinc, and sulfur were studied. The results showed that under the condition of a grinding fineness of 90% with a −0.074 mm fraction, one coarse stage, two fine stages, and two scavenging stages, a copper concentrate with a yield of 4.50%, a copper grade of 18.37%, and a recovery rate of 89.73% was obtained. The gold grade was 4.48 g/t, the gold recovery rate was 34.85%, the silver grade was 109.00 g/t, and the silver recovery rate was 45.42%, meeting the pricing standards.A zinc concentrate with a yield of 3.77%, a zinc grade of 50.57%, and a recovery rate of 83.95% was obtained from one coarse stage, two fine stages, and one scavenging stage. A sulfur concentrate with a yield of 31.78%, a sulfur grade of 48.25%, and a recovery rate of 80.57% was obtained from one coarse stage, one fine stage, and one scavenging stage. The separation and recovery of copper, zinc, and sulfur resources were achieved quite well. Under low alkalinity conditions, copper separation and inhibition of high sulfur were realized, significantly improving the recovery rate of gold and silver in the copper concentrate; ammonium bicarbonate and sulfuric acid were used as a combined activation agent for pyrite in a high−calcium high−alkalinity system, significantly reducing the dosage of sulfuric acid. Therefore, for this high−sulfur complex and difficult−to−select copper−zinc ore deposit, the copper−zinc sulfur priority flotation process is stable and reliable, and has strong adaptability to the ore, providing technical reference for the design of the processing plant's final process.