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Graphite recovery from waste Li-ion battery black mass for direct re-use.

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Title: Graphite recovery from waste Li-ion battery black mass for direct re-use.
Authors: Chernyaev, Alexander1 (AUTHOR), Kobets, Anna2 (AUTHOR), Liivand, Kerli3 (AUTHOR), Tesfaye, Fiseha4,5 (AUTHOR), Hannula, Pyry-Mikko6 (AUTHOR), Kallio, Tanja2 (AUTHOR), Hupa, Leena4 (AUTHOR), Lundström, Mari1 (AUTHOR) mari.lundstrom@aalto.fi
Source: Minerals Engineering. Mar2024, Vol. 208, pN.PAG-N.PAG. 1p.
Subjects: Waste recycling, Lithium-ion batteries, Energy dispersive X-ray spectroscopy, Electric vehicle batteries, Electric vehicles
Abstract: • Black mass was leached and residue pyrolyzed. • Organic impurities were removed in pyrolysis. • Inorganic impurities remained in residue. • Graphite-rich residue performed efficiently as anode in new cell. • Efficient way of graphite recovery from waste Li-ion is proposed. Graphite was recovered from two leached (H 2 SO 4 = 2 M, 60 °C, t = 3 h, Fe3+ = 2 g/L) Li-ion battery black mass concentrates with minimized energy consumption. One black mass originated from a mixture of mobile device and power tool batteries, and another from a single electric vehicle battery. The leach residues were pyrolyzed (800 °C, t = 1 h, Ar atmosphere) to remove the polyvinylidene fluoride (PVDF) binder and other non-metallic fractions. The black mass, its leach residue, and pyrolyzed residue were characterized using inductively coupled plasma-optical emission spectrometry (ICP-OES), ion chromatography (IC), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), Raman spectroscopy, and N 2 adsorption/desorption. After hydrometallurgical recycling and pyrolysis, the main post-metallurgical black mass impurities were cobalt oxide, iron, acid-resistant boehmite (AlO(OH)), and silicon dioxide. The pyrolysis resulted in electrolyte and binder removal, affected the crystallinity of the remaining boehmite. The recovered graphite-rich residue with impurities identified was tested as an anode in half-cells vs. metal Li. The average specific capacities of recovered graphite-rich residues from both sources were 350 and 250 mAh/g at 0.1C and their capacity retention after 100 cycles was high (80 %) suggesting rather slow deterioration and hence the proposed recycling route being promising for the graphite reuse in new Li-ion batteries. [ABSTRACT FROM AUTHOR]
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Database: Engineering Source
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Abstract:• Black mass was leached and residue pyrolyzed. • Organic impurities were removed in pyrolysis. • Inorganic impurities remained in residue. • Graphite-rich residue performed efficiently as anode in new cell. • Efficient way of graphite recovery from waste Li-ion is proposed. Graphite was recovered from two leached (H 2 SO 4 = 2 M, 60 °C, t = 3 h, Fe3+ = 2 g/L) Li-ion battery black mass concentrates with minimized energy consumption. One black mass originated from a mixture of mobile device and power tool batteries, and another from a single electric vehicle battery. The leach residues were pyrolyzed (800 °C, t = 1 h, Ar atmosphere) to remove the polyvinylidene fluoride (PVDF) binder and other non-metallic fractions. The black mass, its leach residue, and pyrolyzed residue were characterized using inductively coupled plasma-optical emission spectrometry (ICP-OES), ion chromatography (IC), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS), X-ray diffraction (XRD), thermogravimetric analysis (TGA), Raman spectroscopy, and N 2 adsorption/desorption. After hydrometallurgical recycling and pyrolysis, the main post-metallurgical black mass impurities were cobalt oxide, iron, acid-resistant boehmite (AlO(OH)), and silicon dioxide. The pyrolysis resulted in electrolyte and binder removal, affected the crystallinity of the remaining boehmite. The recovered graphite-rich residue with impurities identified was tested as an anode in half-cells vs. metal Li. The average specific capacities of recovered graphite-rich residues from both sources were 350 and 250 mAh/g at 0.1C and their capacity retention after 100 cycles was high (80 %) suggesting rather slow deterioration and hence the proposed recycling route being promising for the graphite reuse in new Li-ion batteries. [ABSTRACT FROM AUTHOR]
ISSN:08926875
DOI:10.1016/j.mineng.2024.108587