Preparation of LiCoO2 cathode materials from spent lithium ion batteries are presented. The processes contain reduction, separation, precipitation, regeneration. The optimum conditions of recovery are: the calcination temperature is 500°C, the volume rate of sulfuric acid and the water reaches 0.375, the hightest leach-ing rate of cobalt is 43.53%. According to the solubility of oxalate, ammonium oxalate is choiced as precipitation agent. The investigation of X-ray diffraction (XRD), scanning electron microscopy (SEM), charge-discharge testes at voltage ranges rate from 2.8V to 4.2V versus Li , 0.2 C rate are performed. The results reveal that the regenerative LiCoO2 is pure phase, initial discharge capacity is 128.63 mAh•g-1, after 50 cycles the discharge capacity is 118.61 mAh•g-1, capacity retention rate is 92.21%. The regenerative LiCoO2 exhibits excellent electrochemical performance and stability. The materials may find promising applications in lithium ion batteries.