A new extraction process suitable for treating refractory CuCo 2 S 4 under atmospheric pressure acidic leaching conditions was inv estigated. The effect of variables such as oxidant species, liquid-to-solid ratio, leaching time, oxidizing agent and mineral quality ratio, H 2 SO 4 concentration, temperature and sodium chloride concentration on the extraction efficiency of Co, Cu and Fe from CuCo 2 S 4 were investigated. Under optimal conditions including P 80 -P 90 of the sample was d < 0.0074 mm, stirring speed of 400 rpm, leaching time of 8 h with sodium chlorate (NaClO 3 ) and mineral quality ratio of 0.5, 2 mol/L H 2 SO 4 , liquid-to-solid ratio of 7, leaching temperature of 90°C and 4 mol/L s odium chloride. The leaching efficiency of Co, Cu, and Fe were nearly 97.08%, 100%, and 92.45%, respectively. Furthermore, the contents of cobalt and copper in leaching residue were all less than 0.4 wt.%, which satisfies the requirements of industrial production.