| Summary: | A hydrophobic deep eutectic solvent (HDES) composed of Aliquat 336, decanoic acid, and n-hexanol, diluted with kerosene, was investigated for the selective leaching of LiNi<sub>0.33</sub>Mn<sub>0.33</sub>Co<sub>0.33</sub>O<sub>2</sub> (NMC-111) cathode materials. While conventional choline chloride-based DESs co-dissolve Li and transition metals almost completely, the present HDES–acid hybrid system deliberately sacrifices maximum recovery to achieve selectivity. In combination with a low concentration of H<sub>2</sub>SO<sub>4</sub>, the HDES enabled preferential dissolution of Co and Ni (~84% and ~80% after 6 h at 90 °C, respectively), while Li and Mn largely remained in the solid residue (>93%). Kinetic modeling indicated that the process is controlled by a surface chemical reaction with apparent activation energies of ~~49 kJ mol<sup>−1</sup> (for Ni recovery) and ~51 kJ mol<sup>−1</sup> (for Co recovery). The leaching residues were enriched in stable Li-Mn-O phases in a way that offers a basis for stepwise recovery. These findings show that hydrophobic eutectic media coupled with mild acid activation provide a sustainable pathway for the selective recycling of LIB cathodes.
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