Abstract: Iron ore is the dominant resource in Shandong Province, and a large amount of associated Cu-Co resources cannot be effectively recovered, resulting in waste of resources. In order to improve the comprehensive utilization rate for enterprises, increase the added value of products, and improve the safety of China’s strategic mineral Cu-Co supply chain, this paper uses a Cu-Co mixed rougher concentrate of an iron mine in Shandong Province as a raw material to carry out Cu-Co separation test. On the basis of the process mineralogy research, the optimum process is determined as “Cu-Co mixed flotation-Cu-Co separation” process by carrying out the condition test of roughing dispersant, inhibitor, collector and Cu-Co separation inhibitor. Cu-Co in the raw materials is increased from 2.93% and 0.13% to 23.42% and 0.37%, respectively, by the optimal separation process. The process mineralogy study shows that the copper minerals in the original sample are mainly chalcopyrite and blue chalcocite, and there are trace amounts of chalcocite, bornite, covellite, natural copper and so on. Most of Co exists in pyrite in the form of homomorphism, and a small amount occurs in magnetite and limonite. Cu-Co mixed concentrate is obtained by “one roughing flotation, one scavenging flotation and two concentrating flotation”. Using Z-200 as the collector, the collection effect is the best; using CaO as inhibitor, the separation effect is better. Then copper concentrate and cobalt concentrate are obtained by one “roughing flotation, one scavenging flotation and two concentrating flotation” of Cu-Co mixed concentrate. The grade of Cu in copper concentrate is 23.42%, the recovery rate is 87.68%, the grade of Co is 0.240%, the recovery rate is 19.02%. The grade of Co in cobalt concentrate is 0.370%, the recovery rate is 74.44%, the grade of Cu is 0.53%, the recovery rate is 4.91%. Copper minerals are easy to be separated by flotation, and the existence of isomorphic cobalt limits the grade and recovery of cobalt concentrate, which needs to be further strengthened in the follow-up study. In this study, under the premise of obtaining high copper concentrate grade, the comprehensive utilization of associated cobalt is studied, and the recovery rate of associated elements copper and cobalt is significantly improved.