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Industrial & Engineering Chemistry Research with lower Mg2+ concentrations, that is, from 0 to 0.05 M, confirmed the high impact of Mg2+ on Li2CO3(s) purity that was ∼60% even at a Mg2+ concentration of 0.05 M, caused by the low solubility of Mg carbonate species. In the case of the NaOH and CO2 insufflation precipitation route, a two-step precipitation process was implemented. First, NaOH solution was added, raising the pH and leading to the precipitation of Mg insoluble salts, and then, CO2 was insufflated in the filtered solution. The method was found to be very effective: high Li+ recovery (∼70%) and high Li2CO3(s) purity (∼80%) were obtained even starting with a 0.20 M MgCl2 solution. Li2CO3(s)puritywassuccessfullyenhancedinseveralcases by employing an ethanol washing step that allowed to reach solid purity values of ∼99% accompanied, however, by a Li loss of about 10−20%. Overall,theresultsprovideimportantguidelinesforthebest choice of operational conditions and process control for industrial scale-up of Li+ recovery from relatively low- concentration brines. Specifically, it was demonstrated that precipitation should be performed at a high temperature (80 °C) to decrease Li2CO3 solubility, thus achieving higher recovery values. NaCl and KCl salts can be employed to increase Li recovery, thanks to the induced salting-out effect. On the other hand, a purity decrease is expected, requiring a further purification step. Divalent ions should be removed before precipitation due to the low solubility of their carbonate and hydroxide compounds that precipitate using both Na2CO3 and NaOH solutions. Sulfate ions should be reduced as much as possible before precipitation since they cause a Li2CO3 solubility increase (salting-in) and a kinetic delay effect. In regard to process control, care must be taken for the accurate control of the pH, especially in the case of the NaOH and CO2 precipitation route. In this case, CO2 insufflation must be blocked before re-carbonation of Li2CO3. It is worth noting that the NaOH and CO2 insufflation precipitation route represents an appealing potential industrial application, as also discussed in Section 3.4, whose performance is going to be demonstrated on a pilot scale, in the second phase of the SEArcularMINE project, treating real Li-rich brines. pubs.acs.org/IECR Article ■ ASSOCIATED CONTENT sı Authors Giuseppe Battaglia − Dipartimento di Ingegneria, Università degli Studi di Palermo (UNIPA), Palermo 90128, Italy; orcid.org/0000-0001-8094-0710 Leon Berkemeyer − Fraunhofer Institute for Solar Energy Systems ISE, Freiburg 79110, Germany José Luis Cortina − Chemical Engineering Department, Escola d′Enginyeria de Barcelona Est (EEBE), Universitat Politec̀nicadeCatalunya(UPC)-BarcelonaTECH,Barcelona 08930, Spain; orcid.org/0000-0002-3719-5118 Marc Fernandez de Labastida − Chemical Engineering Department, Escola d′Enginyeria de Barcelona Est (EEBE), UniversitatPolitec̀nicadeCatalunya(UPC)- BarcelonaTECH, Barcelona 08930, Spain Julio Lopez Rodriguez − Chemical Engineering Department, Escola d′Enginyeria de Barcelona Est (EEBE), Universitat Politec̀nicadeCatalunya(UPC)-BarcelonaTECH,Barcelona 08930, Spain Complete contact information is available at: https://pubs.acs.org/10.1021/acs.iecr.2c01397 Author Contributions G.B.: conceptualization, validation, data curation, writing� original draft, writing�review and editing, visualization, and supervision. L.B.: conceptualization, methodology, validation, investigation, data curation, writing�original draft, and visualization. A.C.: conceptualization, methodology, writing� review and editing, project administration, and funding acquisition. J.L.C.: conceptualization, review and editing, supervision, and project administration. M.F.d.L.: method- ology, review and editing. J.L.R.: conceptualization, review, and editing. D.W.: conceptualization, methodology, validation, investigation, resources, data curation, writing�review and editing, visualization, supervision, and project administration. Notes T■he authors declare no competing financial interest. ACKNOWLEDGMENTS This project has received funding from the European Union’s Horizon 2020 research and innovation program under grant agreement no. 869467 (SEArcularMINE). This output reflects only the author’s view. The European Health and Digital Executive Agency (HaDEA) and the European Commission cannot be held responsible for any use that may be made of the i■nformation contained therein. REFERENCES (1) Bello, A. S.; Zouari, N.; Da’ana, D. A.; Hahladakis, J. N.; Al- Ghouti, M. A. An Overview of Brine Management: Emerging Desalination Technologies, Life Cycle Assessment, and Metal Recovery Methodologies. J. Environ. Manage. 2021, 288, 112358. (2) Kumar, A.; Naidu, G.; Fukuda, H.; Du, F.; Vigneswaran, S.; Drioli, E.; Lienhard, J. H. Metals Recovery from Seawater Desalination Brines: Technologies, Opportunities, and Challenges. ACS Sustain. Chem. Eng. 2021, 9, 7704−7712. (3) Al-Absi, R. S.; Abu-Dieyeh, M.; Al-Ghouti, M. A. Brine Management Strategies, Technologies, and Recovery Using Adsorp- tion Processes. Environ. Technol. Innovat. 2021, 22, 101541. (4) Pramanik, B. K.; Nghiem, L. D.; Hai, F. I. Extraction of Strategically Important Elements from Brines: Constraints and Opportunities. Water Res. 2020, 168, 115149. (5) Loganathan, P.; Naidu, G.; Vigneswaran, S. Mining Valuable Minerals from Seawater: A Critical Review. Environ. Sci.: Water Res. Technol. 2017, 3, 37−53. https://doi.org/10.1021/acs.iecr.2c01397 * Supporting Information The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acs.iecr.2c01397. Fundamentals of Li2CO3(s) precipitation routes by Na2CO3 or NaOH/CO2 addition along with tables reporting details of the experimental tests discussed in the main text (PDF) ■ AUTHOR INFORMATION Corresponding Authors Andrea Cipollina − Dipartimento di Ingegneria, Università degli Studi di Palermo (UNIPA), Palermo 90128, Italy; orcid.org/0000-0003-0570-195X; Email: andrea.cipollina@unipa.it Daniel Winter − Fraunhofer Institute for Solar Energy Systems ISE, Freiburg 79110, Germany; Email: daniel.winter@ ise.fraunhofer.de 13601 Ind. Eng. Chem. Res. 2022, 61, 13589−13602PDF Image | Recovery of Lithium Carbonate from Dilute Li Rich Brine
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