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Carbothermal reduction roasting is an important medium-temperature pyrometallurgical process for efficiently recovering valuable elements from spent lithium-ion batteries (LIBs). In this study, combined carbothermal reduction−acetic acid leaching was proposed, aiming to stepwisely recover Li, Ni, Co, and Mn from spent ternary LIBs containing lithium nickel cobalt manganese oxide (LiNixCoyMnzO2, NCM). The biomass waste materials, chitosan, and chitin were chosen as sustainable reducing agents for carbothermal reduction roasting. The synergistic effect of the reducing gases and biochar produced during pyrolysis led to the reduction of transition metals in NCM into Ni, Co, and MnO, separately. Meanwhile, lithium reacted with CO2 to form Li2CO3. Additionally, an acetic acid leaching process was employed to treat the roasting slag, achieving selective leaching of Li and Mn with leaching efficiencies of 98.45% for Li, 1.20% for Ni, 3.10% for Co, and 98.43% for Mn under optimal conditions. Compared to traditional carbothermal reduction roasting methods, this approach used extracts from shrimp/crab shell solid waste as a source of reducing atmosphere and biochar. More importantly, the leaching behaviors of Li, Ni, Co, and Mn were also investigated. Li and Mn were subsequently recovered as lithium carbonate (Li2CO3) and manganese carbonate (MnCO3), respectively. An economic evaluation was also conducted to present a promising strategy for efficiently recycling valuable metals from spent LIBs.

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  This document is the Accepted Manuscript version of a Published Work that appeared in final form in Industrial & Engineering Chemistry Research, copyright © 2025 American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see https://doi.org/10.1021/acs.iecr.4c03579.

Keyword: Recovery of spent electrode materials, Carbothermal reduction, Acid leaching

Date published: 2025-02-12

Publisher: American Chemical Society (ACS)

Journal:

• Industrial & Engineering Chemistry Research (ISSN: 08885885) vol. 64 issue. 6 p. 3453-3464

Funding:

• Natural Science Foundation of Henan Province 242300421222
• National Natural Science Foundation of China 52104271
• Key Laboratory of Metallurgical Emission Reduction & Resources Recycling, Anhui University of Technology JKF24-02
• Zhongyuan Critical Metals Laboratory, Zhengzhou University GJJSGFYQ202416

Manuscript type: Author's version (Accepted manuscript)

MDR DOI: https://doi.org/10.48505/nims.5393

First published URL: https://doi.org/10.1021/acs.iecr.4c03579

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Updated at: 2026-01-28 16:30:04 +0900

Published on MDR: 2026-01-28 14:15:39 +0900