{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,9,18]],"date-time":"2026-09-18T09:34:11Z","timestamp":1789724051599,"version":"4.0.1"},"reference-count":31,"publisher":"MDPI AG","issue":"11","license":[{"start":{"date-parts":[[2023,5,23]],"date-time":"2023-05-23T00:00:00Z","timestamp":1684800000000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"funder":[{"name":"European Regional Development Fund","award":["Interreg V-A Spain-Portugal Program (POCTEP) 2014\u20132020"],"award-info":[{"award-number":["Interreg V-A Spain-Portugal Program (POCTEP) 2014\u20132020"]}]}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Materials"],"abstract":"<jats:p>This study examined how pH hydrolysis affects the recovery process for antimony extracted from spent electrolytes. Various OH\u2212 reagents were used to adjust the pH levels. The findings reveal that pH plays a crucial role in determining the optimal conditions for extracting antimony. The results show that NH4OH and NaOH are more effective compared to water, with optimal conditions at pH 0.5 for water and pH 1 for NH4OH and NaOH, resulting in average antimony extraction yields of 90.4%, 96.1%, and 96.7%, respectively. Furthermore, this approach helps to improve both crystallography and purity related to recovered antimony samples obtained through recycling processes. The solid precipitates obtained lack a crystalline structure, making it difficult to identify the compounds formed, but element concentrations suggest the presence of oxychloride or oxide compounds. Arsenic is incorporated into all solids, affecting the purity of the product, and water showing higher antimony content (68.38%) and lower arsenic values (8%) compared to NaOH and NH4OH. Bismuth integration into solids is less than arsenic (less than 2%) and remains unaffected by pH levels except in tests with water, where a bismuth hydrolysis product is identified at pH 1, accounting for the observed reduction in antimony extraction yields.<\/jats:p>","DOI":"10.3390\/ma16113918","type":"journal-article","created":{"date-parts":[[2023,5,24]],"date-time":"2023-05-24T01:29:26Z","timestamp":1684891766000},"page":"3918","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":10,"title":["Effect of pH Hydrolysis on the Recovery of Antimony from Spent Electrolytes from Copper Production"],"prefix":"10.3390","volume":"16","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-5716-8862","authenticated-orcid":false,"given":"Eduardo","family":"D\u00edaz Guti\u00e9rrez","sequence":"first","affiliation":[{"name":"Departamento de Ingenier\u00eda y Ciencia de los Materiales y del Transporte, Escuela Polit\u00e9cnica Superior, Calle Virgen de \u00c1frica 7, 41011 Seville, Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jos\u00e9 Antonio","family":"Maldonado Calvo","sequence":"additional","affiliation":[{"name":"Atlantic Copper, S.L.U., Francisco Montenegro Avenue, 21001 Huelva, Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jos\u00e9 Mar\u00eda","family":"Gallardo Fuentes","sequence":"additional","affiliation":[{"name":"Departamento de Ingenier\u00eda y Ciencia de los Materiales y del Transporte, Escuela Polit\u00e9cnica Superior, Calle Virgen de \u00c1frica 7, 41011 Seville, Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Antonio","family":"Pa\u00fal Escolano","sequence":"additional","affiliation":[{"name":"Departamento de Ingenier\u00eda y Ciencia de los Materiales y del Transporte, Escuela Polit\u00e9cnica Superior, Calle Virgen de \u00c1frica 7, 41011 Seville, Spain"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2023,5,23]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"253","DOI":"10.1146\/annurev-matsci-070218-010057","article-title":"Challenges of the Circular Economy: A Material, Metallurgical, and Product Design Perspective","volume":"49","author":"Reuter","year":"2019","journal-title":"Annu. Rev. Mater. Res."},{"key":"ref_2","unstructured":"EU Commission (2023, March 10). The Raw Materials Initiative\u2014Meeting Our Critical Needs for Growth and Jobs. Available online: https:\/\/ec.europa.eu\/growth\/sectors\/raw-materials\/policy-strategy_en."},{"key":"ref_3","unstructured":"Blengini, G.A., El Latunussa, C., Eynard, U., Torres De Matos, C., Wittmer, D., Georgitzikis, K., Pavel, C., Carrara, S., Mancini, L., and Unguru, M. (2023, March 15). Study on the EU\u2019s list of Critical Raw Materials (2020) Final Report. Available online: https:\/\/op.europa.eu\/en\/publication-detail\/-\/publication\/c0d5292a-ee54-11ea-991b-01aa75ed71a1\/language-en."},{"key":"ref_4","doi-asserted-by":"crossref","unstructured":"Lewicka, E., Guzik, K., and Galos, K. (2021). On the Possibilities of Critical Raw Materials Production from the EU\u2019s Primary Sources. Resources, 10.","DOI":"10.3390\/resources10050050"},{"key":"ref_5","unstructured":"Ruiz, I., Rios, G., Arbizu, C., Burke, I., and Hanschke, U. (2013). Proceedings of European Metallurgy Congress 2013, GDMB."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"285","DOI":"10.1016\/j.hydromet.2017.06.009","article-title":"Optimizing operating conditions in an ion-exchange column treatment applied to the removal of Sb and Bi impurities from an electrolyte of a copper electro-refining plant","volume":"171","author":"Ruiz","year":"2017","journal-title":"Hydrometallurgy"},{"key":"ref_7","unstructured":"Anderson, C. (2019). SME Mineral Processing and Extractive Metallurgy Handbook, Society for Mining, Metallurgy and Exploration."},{"key":"ref_8","unstructured":"Klochko, K. (2023, March 01). Antimony Data Sheet\u2014Mineral Commodity Summaries 2021, No. 703, pp. 2020\u20132021, 2021, Available online: https:\/\/pubs.usgs.gov\/periodicals\/mcs2021\/mcs2021-antimony.pdf."},{"key":"ref_9","doi-asserted-by":"crossref","first-page":"246","DOI":"10.1016\/j.electacta.2017.09.136","article-title":"Hydrothermal synthesis of antimony oxychlorides submicron rods as anode materials for lithium-ion batteries and sodium-ion batteries","volume":"254","author":"Xie","year":"2017","journal-title":"Electrochimica Acta"},{"key":"ref_10","doi-asserted-by":"crossref","first-page":"169","DOI":"10.1515\/nanoph-2017-0061","article-title":"Emerging technologies for high performance infrared detectors","volume":"7","author":"Tan","year":"2017","journal-title":"Nanophotonics"},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"16166","DOI":"10.1039\/D0TA05433J","article-title":"A critical review on bismuth and antimony halide based perovskites and their derivatives for photovoltaic applications: Recent advances and challenges","volume":"8","author":"Jin","year":"2020","journal-title":"J. Mater. Chem. A"},{"key":"ref_12","doi-asserted-by":"crossref","first-page":"2003172","DOI":"10.1002\/advs.202003172","article-title":"Efficient and Stable Antimony Selenoiodide Solar Cells","volume":"8","author":"Nie","year":"2021","journal-title":"Adv. Sci."},{"key":"ref_13","doi-asserted-by":"crossref","unstructured":"Ling, H., Malfliet, A., Blanpain, B., and Guo, M. (2022). A review of the technologies for antimony recovery from refractory ores and metallurgical residues. Miner. Process. Extr. Met. Rev., 1\u201325.","DOI":"10.1080\/08827508.2022.2132946"},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"107304","DOI":"10.1016\/j.mineng.2021.107304","article-title":"Technological trends, emerging applications and metallurgical strategies in antimony recovery from stibnite","volume":"175","author":"Dembele","year":"2021","journal-title":"Miner. Eng."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"79","DOI":"10.1007\/s40831-016-0043-y","article-title":"Antimony Recovery from End-of-Life Products and Industrial Process Residues: A Critical Review","volume":"2","author":"Dupont","year":"2016","journal-title":"J. Sustain. Met."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"3","DOI":"10.1016\/j.chemer.2012.04.001","article-title":"The metallurgy of antimony","volume":"72","author":"Anderson","year":"2012","journal-title":"Geochemistry"},{"key":"ref_17","doi-asserted-by":"crossref","unstructured":"Speight, J.G. (2018). Hydrolysis. React. Mech. Environ. Eng., 203\u2013229.","DOI":"10.1016\/B978-0-12-804422-3.00006-7"},{"key":"ref_18","first-page":"127","article-title":"Thermodynamic equilibrium of sb-cl-h2o system\u00ae","volume":"7","author":"Ruirong","year":"1997","journal-title":"Trans. Nonferrous Met. Soc. China"},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"2746","DOI":"10.1016\/S1003-6326(16)64370-4","article-title":"Theoretical simulation and experimental study of hydrolysis separation of SbCl3 in complexation\u2013precipitation system","volume":"26","author":"Tian","year":"2016","journal-title":"Trans. Nonferrous Met. Soc. China"},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"1624","DOI":"10.2320\/matertrans.44.1624","article-title":"Hydrolysis of Antimony(III)-Hydrochloric Acid Solution at 25 \u00b0C","volume":"44","author":"Hashimoto","year":"2003","journal-title":"Mater. Trans."},{"key":"ref_21","doi-asserted-by":"crossref","first-page":"115753","DOI":"10.1016\/j.seppur.2019.115753","article-title":"Selective separation of antimony from a Sb-Fe mixed solution by hydrolysis and application in the hydrometallurgical process of antimony extraction","volume":"228","author":"Ye","year":"2019","journal-title":"Sep. Purif. Technol."},{"key":"ref_22","doi-asserted-by":"crossref","first-page":"2127","DOI":"10.1016\/j.jssc.2008.04.043","article-title":"Hydrothermal synthesis of antimony oxychloride and oxide nanocrystals: Sb4O5Cl2, Sb8O11Cl2, and Sb2O3","volume":"181","author":"Chen","year":"2008","journal-title":"J. Solid State Chem."},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"5074","DOI":"10.1021\/acssuschemeng.0c09073","article-title":"Antimony Recovery from Lead-Rich Dross of Lead Smelter and Conversion into Antimony Oxide Chloride (Sb4O5Cl2)","volume":"9","author":"Palden","year":"2021","journal-title":"ACS Sustain. Chem. Eng."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"1943","DOI":"10.1039\/D0AY00148A","article-title":"Arsenic and antimony speciation analysis in copper electrolyte by liquid chromatography coupled to hydride generation atomic fluorescence spectrometry (HPLC-HG-AFS)","volume":"12","author":"Torres","year":"2020","journal-title":"Anal. Methods"},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"110","DOI":"10.1016\/j.hydromet.2010.08.008","article-title":"The removal of antimony from copper electrolytes using amino-phosphonic resins: Improving the elution of pentavalent antimony","volume":"105","author":"Riveros","year":"2010","journal-title":"Hydrometallurgy"},{"key":"ref_26","doi-asserted-by":"crossref","unstructured":"Smith, R.M., and Martell, A.E. (1976). Critical stability constant. Inorg. Complexes, 4.","DOI":"10.1007\/978-1-4757-5506-0"},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"317","DOI":"10.1179\/cmq.2008.47.3.317","article-title":"Bismuth Recovery from Hydrochloric Acid Solution","volume":"47","author":"Kim","year":"2008","journal-title":"Can. Met. Q."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"178","DOI":"10.37358\/RC.20.6.8182","article-title":"Hydrolysis Mechanism of Bismuth in Chlorine Salt System Calculated by Density Functional Method","volume":"71","author":"Chunfa","year":"2020","journal-title":"Rev. de Chim."},{"key":"ref_29","unstructured":"Tooth, B. (2013). The Hydrothermal Chemistry of Bismuth and The Liquid Bismuth Collector Model. [Ph.D. Thesis, University of Adelaide]. Available online: www.lab-initio.com."},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"79","DOI":"10.1016\/0011-9164(95)00089-5","article-title":"An overview of arsenic removal processes","volume":"103","author":"Kartinen","year":"1995","journal-title":"Desalination"},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"9","DOI":"10.1179\/cmq.2008.47.1.9","article-title":"Behaviour of Antimony and Bismuth in Copper Electrorefining Circuits","volume":"47","author":"Beauchemin","year":"2008","journal-title":"Can. Met. Q."}],"container-title":["Materials"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1996-1944\/16\/11\/3918\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,10]],"date-time":"2025-10-10T19:40:35Z","timestamp":1760125235000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1996-1944\/16\/11\/3918"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2023,5,23]]},"references-count":31,"journal-issue":{"issue":"11","published-online":{"date-parts":[[2023,6]]}},"alternative-id":["ma16113918"],"URL":"https:\/\/doi.org\/10.3390\/ma16113918","relation":{},"ISSN":["1996-1944"],"issn-type":[{"value":"1996-1944","type":"electronic"}],"subject":[],"published":{"date-parts":[[2023,5,23]]}}}