Abstract: Process mineralogy of copper-cobalt oxidized ore in Congo has been studied by multiple methods such as advanced instrμment—AMICS (Advanced Mineral Identification and Characterization System) and scanning electron microscope, which points out the mineralogical factors affecting the acid leaching of copper and cobalt. The results show that the oxidation ratio of copper is 92.22%, mainly in malachite and cornetite; the oxidation ratio of cobalt is 85.84%, mainly in heterogenite. The size distribution of copper and cobalt minerals in the ore is uneven, among which copper minerals are mainly mediμm-coarse, cobalt minerals are mainly mediμm-fine, and there are many clay minerals. The copper and cobalt minerals are easy to be exposed under the condition of coarse grinding, it is suggested that acid agitation leaching should be adopted for copper and cobalt recovery under proper coarse grinding conditions. 3.69% copper and 9.46% cobalt are distributed in limonite and Fe-Mn hydrated oxide in the adsorption state, and this part of copper and cobalt is difficult to leach, which mainly affects the improvement of leaching rate.