A novel closed‐loop recycling system of mixed organic acid leaching and sol‐gel method re‐synthesis for LiNi0.5Co0.2Mn0.3O2 cathode material is designed. Mixed organic acid solution consisting of 0.4 mol/L DL‐malic acid and 0.1 mol/L ascorbic acid was applied to the leaching procedure. Under optimal conditions (temperature: 70 °C, time: 30 min, slurry density: 20 g/L), the leaching efficiency of Li, Ni, Co, and Mn is 99.06 %, 97.11 %, 96.46 %, and 97.22 %, respectively. DL‐malic acid has a stronger chelate tendency with metal ions in the mixed acid leachate, which is verified by the UV‐Vis spectra and FT‐IR spectra. Without adding extra chelating reagents to the leachate, LiNi0.5Co0.2Mn0.3O2 material is regenerated by the sol‐gel method directly. Electrochemical performances of the re‐synthesized LiNi0.5Co0.2Mn0.3O2 material exhibit an excellent initial charge and discharge capacity of 156.0 mAh g−1 and 145.2 mAh g−1 at 0.2 C, respectively. As an alternative to LIBs recovery, the advantages of this recovery method are low reagents consumption and environmentally benign.
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