Maximizing the sustainable recycling of spent lithium-ion batteries (LIBs) shows economic and environmental significance. This study recovered lithium cobaltate (LiCoO2, LCO) from spent LIBs cathode powder. The recovered LCO was then combined with NaHSO3 to remove refractory organic pollutants of carbamazepine (CBZ) in water. The degradation of CBZ reached 80.0% within 60 min, by 1O2,
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,
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and
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generated in the LCO/NaHSO
3 reaction. The electron transfer between Co (III) and Co (II) was beneficial to the generation of free radicals. The LCO/NaHSO
3 degraded CBZ effectively in both secondary outlet water and tap water. However, high concentrations of inorganic ions (Cl
−, HCO
3 −, HPO
4 2−, SO
4 2−, NO
3 −) and natural organic matter (humic acid, HA) could inhibit the degradation of CBZ. After three cycles, the stability of the LCO/NaHSO
3 system was demonstrated by the maintained high efficiency in the degradation of CBZ. The obtained data indicate that the LCO/NaHSO
3 system holds great application potential in the field of advanced oxidation degradation of pollutants.