A hydrometallurgical leaching process has been developed for recovery of Co and Li from cathode material (LiCoO2) collected from spent LIBs using a mix solution of glucose and phosphoric acid. The spent LiCoO2 before and after leaching process are analyzed by scanning electron microscopy. A leaching rate of about 98% Co and nearly 100% Li is presented with 1.5mol/L phosphoric acid and 0.02mol/L glucose at 80°C in about 2h. During leaching process, glucose was oxidized into monocarboxylic acid with reduction of Co(III) to Co(II). Co in solution was recovered as Co-oxalate after leaching process. Using glucose as reductant to dissolve LiCoO2 with chelating agent of phosphoric acid is achieved here.