Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodology

The recovery of critical materials such as cobalt, nickel, lithium, manganese and even graphite from spent lithium-ion batteries of different applications and compositions, was studied. The black mass samples were characterized by X-ray diffractometry, revealing mixed lithium oxide phases, and metal...

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Autores: Conte Erustes, Naby, Gómez Martín, José María, Muñoz Sánchez, Jesús Ángel, Castro Ruiz, Laura
Tipo de recurso: artículo
Fecha de publicación:2025
País:España
Institución:Universidad Complutense de Madrid (UCM)
Repositorio:Docta Complutense
Idioma:inglés
OAI Identifier:oai:docta.ucm.es:20.500.14352/124824
Acceso en línea:https://hdl.handle.net/20.500.14352/124824
Access Level:acceso abierto
Palabra clave:669
Spent lithium-ion battery
Black mass
Leaching
Recycling
Graphite
Factorial design
Ingeniería química
Materiales
Metalurgia
3303 Ingeniería y Tecnología Químicas
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oai_identifier_str oai:docta.ucm.es:20.500.14352/124824
network_acronym_str ES
network_name_str España
repository_id_str
spelling Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodologyConte Erustes, NabyGómez Martín, José MaríaMuñoz Sánchez, Jesús ÁngelCastro Ruiz, Laura669Spent lithium-ion batteryBlack massLeachingRecyclingGraphiteFactorial designIngeniería químicaMaterialesMetalurgia3303 Ingeniería y Tecnología QuímicasThe recovery of critical materials such as cobalt, nickel, lithium, manganese and even graphite from spent lithium-ion batteries of different applications and compositions, was studied. The black mass samples were characterized by X-ray diffractometry, revealing mixed lithium oxide phases, and metal content was determined by acid digestion. Inorganic acids showed high efficiencies in leaching metals from the black mass for their full dissociation and greater emission of protons into the medium, while organic acids were a more biodegradable and environmentally friendly alternative to treat these batteries with a less toxic and aggressive treatment and good results. Oxalic acid rose as an interesting option for selective lithium recovery (around 80 % of lithium purity). The leach residue was characterized by XRD, identified as graphite with high purity and graphitization degrees up to 96 %. High recovery efficiency of graphite was achieved. A 33 factorial experimental design was created to evaluate the statistical significance of various variables in metal leaching. Time and temperature emerged as the most significant factors, their increase enhanced leaching efficiency, while pulp density showed higher leaching efficiency at intermediate values. Final optimization of acid concentration and H2O2 dosing led to recoveries of 93 % of Co, 98 % of Li, 86 % of Ni and 97 % of Mn, at S/L = 10 g/L, T = 75 °C, t = 24 h, H2O2 = 0.5 g/g, and using 1 N gluconic acid as lixiviant, from a black mass with high cobalt content. The present methodology stands out for its applicability to black mass samples of batteries of different origins (computer, electric vehicle, cordless tool…), a simple and effective approach, easily applicable to existing processes at industrial level. It favors the selection of the best lixiviants for each case while considering environmental, economic and engineering criteria.ElsevierUniversidad Complutense de Madrid20252025-08-0120252025-08-01journal articlehttp://purl.org/coar/resource_type/c_6501VoRhttp://purl.org/coar/version/c_970fb48d4fbd8a85info:eu-repo/semantics/articleapplication/pdfhttps://hdl.handle.net/20.500.14352/124824reponame:Docta Complutenseinstname:Universidad Complutense de Madrid (UCM)Inglésengopen accesshttp://purl.org/coar/access_right/c_abf2Attribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessoai:docta.ucm.es:20.500.14352/1248242026-06-02T12:44:21Z
dc.title.none.fl_str_mv Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodology
title Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodology
spellingShingle Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodology
Conte Erustes, Naby
669
Spent lithium-ion battery
Black mass
Leaching
Recycling
Graphite
Factorial design
Ingeniería química
Materiales
Metalurgia
3303 Ingeniería y Tecnología Químicas
title_short Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodology
title_full Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodology
title_fullStr Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodology
title_full_unstemmed Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodology
title_sort Efficient recovery of strategic materials from spent lithium-ion batteries: Optimization using an experimental design methodology
dc.creator.none.fl_str_mv Conte Erustes, Naby
Gómez Martín, José María
Muñoz Sánchez, Jesús Ángel
Castro Ruiz, Laura
author Conte Erustes, Naby
author_facet Conte Erustes, Naby
Gómez Martín, José María
Muñoz Sánchez, Jesús Ángel
Castro Ruiz, Laura
author_role author
author2 Gómez Martín, José María
Muñoz Sánchez, Jesús Ángel
Castro Ruiz, Laura
author2_role author
author
author
dc.contributor.none.fl_str_mv Universidad Complutense de Madrid
dc.subject.none.fl_str_mv 669
Spent lithium-ion battery
Black mass
Leaching
Recycling
Graphite
Factorial design
Ingeniería química
Materiales
Metalurgia
3303 Ingeniería y Tecnología Químicas
topic 669
Spent lithium-ion battery
Black mass
Leaching
Recycling
Graphite
Factorial design
Ingeniería química
Materiales
Metalurgia
3303 Ingeniería y Tecnología Químicas
description The recovery of critical materials such as cobalt, nickel, lithium, manganese and even graphite from spent lithium-ion batteries of different applications and compositions, was studied. The black mass samples were characterized by X-ray diffractometry, revealing mixed lithium oxide phases, and metal content was determined by acid digestion. Inorganic acids showed high efficiencies in leaching metals from the black mass for their full dissociation and greater emission of protons into the medium, while organic acids were a more biodegradable and environmentally friendly alternative to treat these batteries with a less toxic and aggressive treatment and good results. Oxalic acid rose as an interesting option for selective lithium recovery (around 80 % of lithium purity). The leach residue was characterized by XRD, identified as graphite with high purity and graphitization degrees up to 96 %. High recovery efficiency of graphite was achieved. A 33 factorial experimental design was created to evaluate the statistical significance of various variables in metal leaching. Time and temperature emerged as the most significant factors, their increase enhanced leaching efficiency, while pulp density showed higher leaching efficiency at intermediate values. Final optimization of acid concentration and H2O2 dosing led to recoveries of 93 % of Co, 98 % of Li, 86 % of Ni and 97 % of Mn, at S/L = 10 g/L, T = 75 °C, t = 24 h, H2O2 = 0.5 g/g, and using 1 N gluconic acid as lixiviant, from a black mass with high cobalt content. The present methodology stands out for its applicability to black mass samples of batteries of different origins (computer, electric vehicle, cordless tool…), a simple and effective approach, easily applicable to existing processes at industrial level. It favors the selection of the best lixiviants for each case while considering environmental, economic and engineering criteria.
publishDate 2025
dc.date.none.fl_str_mv 2025
2025-08-01
2025
2025-08-01
dc.type.none.fl_str_mv journal article
http://purl.org/coar/resource_type/c_6501
VoR
http://purl.org/coar/version/c_970fb48d4fbd8a85
dc.type.openaire.fl_str_mv info:eu-repo/semantics/article
format article
dc.identifier.none.fl_str_mv https://hdl.handle.net/20.500.14352/124824
url https://hdl.handle.net/20.500.14352/124824
dc.language.none.fl_str_mv Inglés
eng
language_invalid_str_mv Inglés
language eng
dc.rights.none.fl_str_mv open access
http://purl.org/coar/access_right/c_abf2
Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
dc.rights.openaire.fl_str_mv info:eu-repo/semantics/openAccess
rights_invalid_str_mv open access
http://purl.org/coar/access_right/c_abf2
Attribution-NonCommercial-NoDerivatives 4.0 International
http://creativecommons.org/licenses/by-nc-nd/4.0/
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
dc.source.none.fl_str_mv reponame:Docta Complutense
instname:Universidad Complutense de Madrid (UCM)
instname_str Universidad Complutense de Madrid (UCM)
reponame_str Docta Complutense
collection Docta Complutense
repository.name.fl_str_mv
repository.mail.fl_str_mv
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score 15,81155