The leaching residue after extracting arsenic from the arsenic- nickel/cobalt-residue is treated to recover copper, cobalt and nickel and so on. The experimental results show that the best conditions are as follows: the time is 2 hours, the liquid-solid-ratio is 10:1, the ratio of oxidant to raw material is 0.6 ml/g, the sulfuric acid concentration is 20% and the temperature is 40 °C. Under the above conditions, the leaching ratio of copper, cobalt, nickel, zinc and arsenic are 96.31%, 97.23%, 98.56%, 98.46%, 93.84%, respectively. The leaching kinetics of copper, cobalt and nickel were further studied. The activation energy of copper, cobalt, nickel leaching reaction are 47.22kJ/mol, 37.91 kJ/mol, 44.93 kJ/mol, respectively; and the reaction grade are 1.88, 1.94, 1.92, respectively. In this study, the valuable metals are further recovered in the leaching residue. It is beneficial to the efficient use of resources, reducing resources waste in the metallurgical process.