Hydrometallurgical process for recovery of aluminum, lithium and cobalt from the spent secondary lithium–ion batteries of Yun–lin battery recycle corporation was investigated. The recovery efficiency of spent lithium–ion secondary batteries on the hydrometallurgical process of their leachant concentration, temperature (T), time (t), solid–to–liquid ratio (S:L) were investigated. The experimental procedure include the following three major steps: (1) solvent extraction separation of aluminum by NaOH, (2) solvent extraction separation of lithium and cobalt by 3 mol/L H2SO4 (4.76 % (v/v) 35% (v/v) H2O2) from the final solution after aluminum removal. Finally, (3) cobalt are precipitated by ammonium oxalate ((NH4)2C2O4) from the final solutions after aluminum removal. The experimental results for treating 3 g of anode plus in the battery by this new technique were reported, and some evaluation were also carried out. In the processing, the percent removal of impurities, such as aluminum could reach 90.6% or more, and that of lithium and cobalt were all more than 90.0%.