Abstract: Due to the complex mineral composition of Congo cobalt sulphide copper concentrate and the poor effect of direct acid leaching, the thermal activation pretreatment and sulfuric acid leaching process was investigated to strengthen the recovery of copper and cobalt. The test results showed that the leaching rate of cobalt and copper was 98.51% and 97.80% respectively obtained by the calcine generated from thermal activation at 500℃ for 2 h with the mass ratio of cobalt sulfide copper concentrate, cobalt oxide ore and anhydrous sodium carbonate of 1 GA6FA 3 GA6FA 0.4 reacting for 5 hours under the conditions of the initial concentration of sulfuric acid of 1.25 mol/L, liquid-solid ratio of 5 to 1 mL/g, leaching temperature of 80℃, and the stirring speed of 300 r/min. The process adopted in the experiment can realize the efficient recovery and utilization of cobalt and copper in the cobalt-copper sulfide concentrates.