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This study investigates how common pretreatments for recovering black mass from end-of-life (EoL) electric vehicle (EV) lithium-ion batteries (LIBs) influence graphene oxide (GO) synthesis. Black mass was obtained through (i) industrial-scale carbothermal reduction of whole EV battery packs, (ii) industrial-scale mechanical processing, and (iii) lab-scale mechanochemical treatment via reactive ball milling. Characterizations assessed the impact of these pretreatments, along with conventional acid leaching, on graphite properties such as interlayer spacing, oxidation degree, and defectivity—key factors for potential anode reuse. The mechanochemically treated sample achieved an outstanding GO yield of 92 %, whereas other black masses reached up to 30 %. GO yields were further analysed using the Hummers’ method after acid leaching for metal removal. This approach enhanced yields, reaching 96 % for the mechanochemically treated sample and up to 46 % for the others. The improvements were attributed to reduced reagent consumption and the partial exfoliation and oxidation of graphite during leaching. Additionally, lithium intercalation/deintercalation during battery cycling increased GO yield compared to commercial pristine graphite. These findings highlight mechanochemical pretreatment as a promising strategy to integrate high-yield GO production into LIB recycling workflows.

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The article “Implementation of a sub-and supercritical carbon dioxide process for the selective recycling of the electrolyte from spent Li-ion battery” is available in the “Journal of CO2 Utilization, Volume 81, Elsevier.

Highlights
• Sub- and supercritical CO2 extraction process suitable to selectively extract electrolyte from LiB waste.

• CO2 density significant factor for the selective electrolyte extraction process.

• Full recovery of non-polar electrolyte solvents dimethyl carbonate, and ethyl methyl carbonate.

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The article of the electrochemical extraction of lithium from end-of-life electric vehicle (EV) Li-ion battery black mass has been published in the Journal of Energy Chemistry, ScienceDirect (Elsevier).

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