In this paper, a hydrometallurgical process has been proposed to recover valuable metals from spent lithium-ion batteries in citric acid media. Leaching efficiencies as high as 97%, 95%, 94%, and 99% of Ni, Co, Mn, and Li were achieved under the optimal leaching experimental conditions of citric acid concentration of 2 mol L −1 , leaching temperature of 80 °C, leaching time of 90 min, liquid–solid ratio of 30 ml g −1 , and 2 vol. % H 2 O 2 . For the metals recovery process, nickel and cobalt were selectively precipitated by dimethylglyoxime reagent and ammonium oxalate sequentially. Then manganese was extracted by Na-D2EHPA and the manganese-loaded D2EHPA was stripped with sulfuric acid. The manganese was recovered as MnSO 4 in aqueous phase and D2EHPA could be reused after saponification. Finally, lithium was precipitated by 0.5 mol L −1 sodium phosphate. Under their optimal conditions, the recovery percentages of Ni, Co, Mn, and Li can reach 98%, 97%, 98%, and 89%, respectively. This is a relatively simple route in which all metal values could be effectively leached and recovered in citric acid media.