The paper focuses on the improved process of metal recovery from lithium-ion batteries (LIBs) lithium nickel manganese cobalt oxide (NMC) cathode waste materials by using hydrometallurgical methods. In the acid leaching step, the essential effects of acidity concentration, H 2 O 2 concentration, leaching time, liquid-solid mass ratio, and reaction temperature with the leaching percentage were investigated in detail. The cathode material was leached with 2M H 2 SO 4 and 10 vol. % H 2 O 2 at 70 • C and 300 rpm using a liquid-solid mass ratio of 30 mL/g. In order to complete the recovery process, this paper designs the proper separation process to recover valuable metals. The leach liquor in the recovery process uses Cyanex 272 to first extract Co and Mn to the organic phase. Secondly, Co and Mn are separated by using D2EHPA, and a high purity of Co is obtained. Thirdly, Ni is selectively precipitated by using DMG, and Ni is completely formed as a solid complex. Finally, in the chemical precipitation process, the remaining Li in the leach liquor is recovered as Li 2 CO 3 precipitated by saturated Na 2 CO 3 , and Co, Mn, and Ni are recovered as hydroxides by NaOH. This hydrometallurgical process may provide an effective separation and recovery of valuable metals from LIBs waste cathode materials.