A recycling process including separation of electrode materials by ultrasonic treatment,acid leaching,Fe-removing,precipitation of cobalt,nickel,manganese and lithium has been applied successfully to recycle spent lithium-ion batteries and to synthesize LiNi1/3Co1/3Mn1/3O2. When ultrasonic treatment with 2-nitroso-4-methylphenol（NMP） at 40 ℃ for 15 min,the electrode materials are separated completely. Above 99% of Co,Ni,Mn and Li,95% of Fe in the separated electrodes are acid-leached in the optimized conditions of 2 mol/L H2SO4,1∶2 H2O2-H2SO4（molar ratio）,70 ℃,1∶10 initial S∶L ratio,and 1 h. 99.5% of Fe and less than 1% of Co,Ni,Mn in the leaching solution can be removed in the conditions of initial pH value 2.0-2.5 adjusted by adding 18% Na2CO3,90 ℃ and stirring time 3 h. After adjusted to be equal by adding NiSO4,CoSO4 and MnSO4 solution,97.1% of Ni,Co,Mn in the Fe-removing surplus leaching solution can be recovered as Ni1/3Co1/3Mn1/3（OH）2. 94.5% of Li in the surplus filtrate after the deposition of Co,Ni and Mn can be recovered as Li2CO3. The LiNi1/3Co1/3Mn1/3O2,prepared from the recovered compounds,is found to have good characteristics of the layered structure and elecrtochemical performance.
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