This research aimed at recovering metals retained in the tailings from the flotation of copper (Cu) and cobalt (Co) ores conducted at the New Concentrator in Kipushi (NCK). Metals retention in the tailings (0.73% Cu and 0.37% Co) increased due to the removal of the gravity separation section from the processing circuit together with changes arising in the feed mineralogical characteristics namely the increase in sulfide minerals. The concentrator’s feed was traditionally composed of oxidized minerals of Cu and Co from the Luiswishi deposit (DR Congo). Experiments conducted at the laboratory scale enabled identifying two exploitable routes for recovering metals retained in the tailings: firstly, the sulfuric acid leaching of tailings under reducing conditions in view of preparing a leach liquor (2.43 g/L Cu and 1.10 g/L Co) that can be utilized for cementing Cu, using iron chips and precipitating Co; secondly, the flotation of valuable minerals using xanthates in view of obtaining a rougher concentrate grading 1.43% Cu and 0.75% Co recovered at 56% and 59%, respectively, and later on, the obtaining of a cleaner concentrate assaying 3.97% Cu and 2.4% Co at the recoveries of 35% and 43%, respectively. The final concentrate enables the hydrometallurgical extraction of Cu and Co.