Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion Batteries

The processing and extraction of critical metals from black mass is important to battery recycling. Separation and recovery of critical metals (Co, Ni, Li, and Mn) from other metal impurities must yield purified metal salts, while avoiding substantial losses of critical metals. Solvent extraction in...

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Main Authors: Ayorinde Emmanuel Ajiboye, Trevor L. Dzwiniel
Format: Article
Language:English
Published: MDPI AG 2023-11-01
Series:Batteries
Subjects:
Online Access:https://www.mdpi.com/2313-0105/9/11/549
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author Ayorinde Emmanuel Ajiboye
Trevor L. Dzwiniel
author_facet Ayorinde Emmanuel Ajiboye
Trevor L. Dzwiniel
author_sort Ayorinde Emmanuel Ajiboye
collection DOAJ
description The processing and extraction of critical metals from black mass is important to battery recycling. Separation and recovery of critical metals (Co, Ni, Li, and Mn) from other metal impurities must yield purified metal salts, while avoiding substantial losses of critical metals. Solvent extraction in batch experiments were conducted using mixed metal sulphates obtained from the leach liquor obtained from spent and shredded lithium-ion batteries. Selective extraction of Mn<sup>2+</sup>, Fe<sup>3+</sup>, Al<sup>3+</sup> and Cu<sup>2+</sup> from simulated and real leached mixed metals solution was carried out using di-2-ethylhexylphophoric acid (D2EPHA) and Cyanex-272 at varying pH. Further experiments with the preferred extractant (D2EPHA) were performed under different conditions: changing the concentration of extractant, organic to aqueous ratio, and varying the diluents. At optimum conditions (40% <i>v</i>/<i>v</i> D2EPHA in kerosene, pH 2.5, O:A = 1:1, 25 °C, and 20 min), 85% Mn<sup>2+</sup>, 98% Al<sup>3+</sup>, 100% Fe<sup>3+</sup>, and 43% Cu<sup>2+</sup> were extracted with losses of only trace amounts (<5.0%) of Co<sup>2+</sup>, Ni<sup>2+</sup>, and Li<sup>+</sup>. The order of extraction efficiency for the diluents was found to be kerosene > Exxal-10 >>> dichloromethane (CH<sub>2</sub>Cl<sub>2</sub>) > toluene. Four stages of stripping of metals loaded on D2EPHA were performed as co-extracted metal impurities were selectively stripped, and a purified MnSO<sub>4</sub> solution was produced. Spent extractant was regenerated after Fe<sup>3+</sup> and Al<sup>3+</sup> were completely stripped using 1.0 M oxalic acid (C<sub>2</sub>H<sub>2</sub>O<sub>4</sub>).
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spelling doaj.art-361706d5e11c4cbdb72a65f5151bd87d2023-11-24T14:29:10ZengMDPI AGBatteries2313-01052023-11-0191154910.3390/batteries9110549Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion BatteriesAyorinde Emmanuel Ajiboye0Trevor L. Dzwiniel1Applied Materials Division, Argonne National Laboratory, Lemont, Chicago, IL 60439, USAApplied Materials Division, Argonne National Laboratory, Lemont, Chicago, IL 60439, USAThe processing and extraction of critical metals from black mass is important to battery recycling. Separation and recovery of critical metals (Co, Ni, Li, and Mn) from other metal impurities must yield purified metal salts, while avoiding substantial losses of critical metals. Solvent extraction in batch experiments were conducted using mixed metal sulphates obtained from the leach liquor obtained from spent and shredded lithium-ion batteries. Selective extraction of Mn<sup>2+</sup>, Fe<sup>3+</sup>, Al<sup>3+</sup> and Cu<sup>2+</sup> from simulated and real leached mixed metals solution was carried out using di-2-ethylhexylphophoric acid (D2EPHA) and Cyanex-272 at varying pH. Further experiments with the preferred extractant (D2EPHA) were performed under different conditions: changing the concentration of extractant, organic to aqueous ratio, and varying the diluents. At optimum conditions (40% <i>v</i>/<i>v</i> D2EPHA in kerosene, pH 2.5, O:A = 1:1, 25 °C, and 20 min), 85% Mn<sup>2+</sup>, 98% Al<sup>3+</sup>, 100% Fe<sup>3+</sup>, and 43% Cu<sup>2+</sup> were extracted with losses of only trace amounts (<5.0%) of Co<sup>2+</sup>, Ni<sup>2+</sup>, and Li<sup>+</sup>. The order of extraction efficiency for the diluents was found to be kerosene > Exxal-10 >>> dichloromethane (CH<sub>2</sub>Cl<sub>2</sub>) > toluene. Four stages of stripping of metals loaded on D2EPHA were performed as co-extracted metal impurities were selectively stripped, and a purified MnSO<sub>4</sub> solution was produced. Spent extractant was regenerated after Fe<sup>3+</sup> and Al<sup>3+</sup> were completely stripped using 1.0 M oxalic acid (C<sub>2</sub>H<sub>2</sub>O<sub>4</sub>).https://www.mdpi.com/2313-0105/9/11/549black masscritical metalsextractantsdiluentsseparationstripping
spellingShingle Ayorinde Emmanuel Ajiboye
Trevor L. Dzwiniel
Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion Batteries
Batteries
black mass
critical metals
extractants
diluents
separation
stripping
title Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion Batteries
title_full Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion Batteries
title_fullStr Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion Batteries
title_full_unstemmed Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion Batteries
title_short Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion Batteries
title_sort sequential recovery of critical metals from leached liquor of processed spent lithium ion batteries
topic black mass
critical metals
extractants
diluents
separation
stripping
url https://www.mdpi.com/2313-0105/9/11/549
work_keys_str_mv AT ayorindeemmanuelajiboye sequentialrecoveryofcriticalmetalsfromleachedliquorofprocessedspentlithiumionbatteries
AT trevorldzwiniel sequentialrecoveryofcriticalmetalsfromleachedliquorofprocessedspentlithiumionbatteries