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Keywords = lithium leaching

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20 pages, 6015 KB  
Article
Selective Lithium Extraction via Chlorination Roasting and Subsequent Valuable Metal Leaching from Spent Lithium-Ion Batteries
by Minji Kim, Seungyun Han, Yong Hwan Kim, Young-Min Kim and Eunmi Park
Metals 2025, 15(10), 1085; https://doi.org/10.3390/met15101085 - 29 Sep 2025
Abstract
The rapid growth of the electric vehicle (EV) market has highlighted the critical importance of securing a stable supply chain for lithium-ion battery (LIB) resources, thereby increasing the need for efficient recycling technologies. Among these, lithium recovery remains a major challenge due to [...] Read more.
The rapid growth of the electric vehicle (EV) market has highlighted the critical importance of securing a stable supply chain for lithium-ion battery (LIB) resources, thereby increasing the need for efficient recycling technologies. Among these, lithium recovery remains a major challenge due to significant losses during conventional processes. In this study, a chlorination roasting process was introduced to convert Li2O in spent LIBs into LiCl, which was subsequently evaporated for selective lithium extraction and recovery. Roasting experiments were conducted under air, vacuum, and N2 conditions at 800–1000 °C for 1–5 h, with Cl/Li molar ratios ranging from 0.5 to 8. The optimal condition for lithium evaporation, achieving 100% recovery, was identified as 1000 °C for 5 h, with a Cl/Li molar ratio of 6 under vacuum. Following lithium removal, residual valuable metals were extracted through H2SO4 leaching, and the effects of acid concentration and H2O2 addition on leaching efficiency were examined. The air-roasted samples exhibited the highest leaching performance, while the vacuum- and N2-roasted samples showed relatively lower efficiency; however, the addition of H2O2 significantly enhanced leaching yields in these cases. Full article
(This article belongs to the Section Extractive Metallurgy)
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12 pages, 1446 KB  
Article
Investigation on Li Recovery from Greek Coal Fly Ash Under a Circular Economy Framework: An Experimental Study
by Despina Pentari, Pagona Makri, Panagiotis Xanthopoulos and Despina Vamvuka
Separations 2025, 12(9), 251; https://doi.org/10.3390/separations12090251 - 15 Sep 2025
Viewed by 278
Abstract
Lithium is classified as a critical element and is widely used in a variety of high-tech applications. Within the framework of a circular economy, demand is rising for technologies capable of recovering high-tech metals from waste materials and industrial byproducts. Coal fly ash [...] Read more.
Lithium is classified as a critical element and is widely used in a variety of high-tech applications. Within the framework of a circular economy, demand is rising for technologies capable of recovering high-tech metals from waste materials and industrial byproducts. Coal fly ash (CFA) has attracted significant attention as a promising secondary resource for this purpose. Effective recovery requires the assessment of both metal enrichment levels and the underlying binding and leaching characteristics. The present study aims to contribute to advancing lithium recovery technology using coal fly ash as a secondary resource, thereby promoting waste valorization. Fourteen samples of coal fly ash from different power plants were collected and their mineralogy was studied by X-ray powder diffraction (XRD), their major constituents were analyzed by X-ray fluorescence spectroscopy (XRF), and their Li content was determined by inductively coupled plasma mass spectrometry (ICP-MS). Leaching experiments were conducted for selected samples using mineral acids (HCl and HF) and citric acid. Lithium concentrations in the analyzed samples ranged from 80 to 256 mg/kg, indicating enrichment relative to both global ash averages (enrichment factor > 1) and the Earth’s crust (enrichment factor > 2). Li in the samples, could be mainly associated with the amorphous fraction present in the samples. Leaching behavior across the samples follows a consistent trend, with hydrofluoric acid exhibiting the highest lithium extraction efficiency—reaching up to 79.9%. Full article
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18 pages, 4516 KB  
Article
Mechanochemical Activation as a Key Step for Enhanced Ammonia Leaching of Spent LiCoO2 Cathodes
by Lyazzat Mussapyrova, Bagdatgul Milikhat, Matej Baláž, Aisulu Batkal, Kaster Kamunur and Rashid Nadirov
Metals 2025, 15(9), 1021; https://doi.org/10.3390/met15091021 - 15 Sep 2025
Viewed by 335
Abstract
The growing demand for lithium-ion batteries (LIBs) has led to an urgent need for sustainable recycling strategies for spent cathode materials. In this study, a mechanochemical approach was developed for the recovery of lithium and cobalt from end-of-life LiCoO2 cathodes using high-energy [...] Read more.
The growing demand for lithium-ion batteries (LIBs) has led to an urgent need for sustainable recycling strategies for spent cathode materials. In this study, a mechanochemical approach was developed for the recovery of lithium and cobalt from end-of-life LiCoO2 cathodes using high-energy ball milling. For the first time, aluminum and carbon were employed as internal reducing agents, facilitating the in situ decomposition of LiCoO2 into CoO, Li2O, and metallic Co. X-ray diffraction analysis confirmed significant structural disorder, phase transitions, and the formation of CoO, AlCo, and spinel-like CoAl2O4. The Taguchi method was applied to optimize milling parameters, identifying 800 rpm, 60 min, and a ball-to-powder ratio of 50:1 as the most effective conditions for structural activation. Subsequent ammonia leaching under fixed conditions (3.0 M NH3·H2O, 1.0 M (NH4)2CO3, 60 °C, 25 mL/g, 6 h) demonstrated high recovery efficiencies: up to 94.6% for lithium and 83.7% for cobalt in the best-performing samples. These results highlight the synergistic benefits of mechanical activation and reductant-assisted phase engineering for enhancing metal recovery. The proposed method offers a simple, scalable, and eco-friendly route for the hydrometallurgical recycling of LIB cathodes without requiring extensive chemical pretreatment. Full article
(This article belongs to the Section Extractive Metallurgy)
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17 pages, 2017 KB  
Article
Sustainable Recovery of Critical Metals from Spent Lithium-Ion Batteries Using Deep Eutectic Solvents
by Jafar Goudarzi, Zhi Chen, Gaixia Zhang, Jinguang Hu, Karim Zaghib, Sixu Deng, Afzal Ahmed Dar, Xiaolei Wang, Fariborz Haghighat, Catherine N. Mulligan, Chunjiang An and Antonio Avalos Ramirez
Batteries 2025, 11(9), 340; https://doi.org/10.3390/batteries11090340 - 14 Sep 2025
Viewed by 571
Abstract
The surging demand for lithium-ion batteries (LIBs) has intensified the need for sustainable recovery of critical metals such as lithium, manganese, cobalt, and nickel from spent cathodes. While conventional hydrometallurgical and pyrometallurgical methods are widely used, they involve high energy consumption, hazardous waste [...] Read more.
The surging demand for lithium-ion batteries (LIBs) has intensified the need for sustainable recovery of critical metals such as lithium, manganese, cobalt, and nickel from spent cathodes. While conventional hydrometallurgical and pyrometallurgical methods are widely used, they involve high energy consumption, hazardous waste generation, and complex processing steps, underscoring the urgency of developing eco-friendly alternatives. This study presents a novel, water-enhanced deep eutectic solvent (DES) system composed of choline chloride and D-glucose for the efficient leaching of valuable metals from spent LiMn-based battery cathodes. The DES was synthesized under mild conditions and applied to dissolve cathode powder, with leaching performance optimized by varying temperature and duration. Under optimal conditions (100 °C, 24 h), exceptional recovery efficiencies were achieved: 98.9% for lithium, 98.4% for manganese, and 71.7% for nickel. Material characterization using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), and inductively coupled plasma mass spectrometer (ICP-MS) confirm effective phase dissolution and metal release. Although this DES system requires relatively higher temperature and longer reaction time compared to traditional acid leaching, it offers clear advantages in terms of non-toxicity, biodegradability, and elimination of strong oxidizing agents. These results demonstrate the potential of water-enhanced choline chloride–glucose DES as a green alternative for future development in sustainable battery recycling, supporting circular economy objectives. Full article
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14 pages, 3347 KB  
Article
Leaching Behavior and Mechanisms of Li, Rb, K, Sr, and Mg in Clay-Type Lithium Ore via a Roasting–Water Leaching Process
by Bo Feng, Dong An, Huaigang Cheng, Xiaoou Zhang and Jing Zhao
Minerals 2025, 15(9), 944; https://doi.org/10.3390/min15090944 - 4 Sep 2025
Viewed by 388
Abstract
The extraction of lithium from clay-type lithium ores has attracted significant attention, but the leaching behavior of associated elements, such as Rb, K, and Sr, remains less explored. This study quantitatively investigated the leaching behaviors and mechanisms of Li, Rb, K, Sr, and [...] Read more.
The extraction of lithium from clay-type lithium ores has attracted significant attention, but the leaching behavior of associated elements, such as Rb, K, and Sr, remains less explored. This study quantitatively investigated the leaching behaviors and mechanisms of Li, Rb, K, Sr, and Mg in clay-type lithium ore through water leaching and roasting–water leaching processes. The results show that during direct water leaching, the leaching efficiency of K ranged between 10% and 13%, while Li and Sr exhibited lower extraction rates, requiring prolonged high-temperature leaching. Rb dissolution was minimal, and the leaching efficiency of Mg was significantly affected by temperature. In contrast, roasting–water leaching significantly enhanced the leaching efficiency, achieving extraction rates of 90.65% for Li, 92.91% for Rb, 75.85% for K, and 36.99% for Sr. However, Mg leaching was suppressed to below 1%. Roasting disrupted the original silicate and carbonate lattices, generating new phases that altered the ore’s microstructure into aggregated dense phases and needle-like porous phases upon water leaching, thereby facilitating the release of Li, Rb, K, and Sr. A research finding was that the new phase generated by magnesium inhibited its leaching, which indirectly enhanced subsequent Li, Rb, K, and Sr extraction and separation. These findings provide a quantitative foundation for optimizing multi-element co-extraction from clay-type lithium ores. Full article
(This article belongs to the Section Mineral Processing and Extractive Metallurgy)
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18 pages, 3869 KB  
Article
Selective and Closed-Loop Recycling of Different Metals from Spent Lithium-Ion Batteries Through Phosphoric Acid Leaching: Parameter Optimization and Regulation of Reaction Kinetics
by Linling Guo, Zihao Chen, Yutong Guo, Chaoyang Chen, Yan Wang and Xiangping Chen
Sustainability 2025, 17(17), 7862; https://doi.org/10.3390/su17177862 - 1 Sep 2025
Viewed by 585
Abstract
The sustainable recycling of valuable metals from spent lithium-ion batteries (LIBs) is critical for resource conservation and environmental protection but remains challenging due to the complex coexistence of target and impurity metals. This study systematically investigates the selective leaching behaviors of metals (Co, [...] Read more.
The sustainable recycling of valuable metals from spent lithium-ion batteries (LIBs) is critical for resource conservation and environmental protection but remains challenging due to the complex coexistence of target and impurity metals. This study systematically investigates the selective leaching behaviors of metals (Co, Li, Cu, Fe, Al) in phosphoric acid media, revealing that lithium could be preferentially extracted in mild acidic conditions (0.8 mol/L H3PO4), while complete dissolution of both Li and Co was achieved in concentrated acid (2.0 mol/L H3PO4). Kinetic analysis demonstrated that metal leaching followed a chemically controlled mechanism, with distinct extraction sequences: Li > Cu~Co > Fe > Al in dilute acid and Cu > Al~Li > Fe > Co in concentrated acid. Furthermore, we developed a closed-loop process wherein oxalic acid simultaneously precipitates Co/Li while regenerating H3PO4, enabling acid reuse with minimal efficiency loss during cyclic leaching. These findings establish a single-step phosphoric acid leaching strategy for selective metal recovery, governed by tunable acid concentration and reaction kinetics, offering a sustainable pathway for LIBs recycling. Full article
(This article belongs to the Section Waste and Recycling)
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20 pages, 6138 KB  
Article
Sequential Redox Precipitation and Solvent Extraction for Comprehensive Metal Recovery from Spent High Manganese Lithium-Ion Battery
by Jiawei Zhang, Fupeng Liu, Chunfa Liao, Tao Zhang, Feixiong Chen, Hao Wang and Yuxin Gao
Metals 2025, 15(9), 948; https://doi.org/10.3390/met15090948 - 26 Aug 2025
Viewed by 609
Abstract
The traditional recycling process of spent lithium-ion battery(LIB) with high Mn content faces the defects of high cost of neutralization and precipitation, poor economics of Mn extraction, and serious Li loss. Therefore, this paper introduces a comprehensive hydrometallurgical method for extracting valuable metals [...] Read more.
The traditional recycling process of spent lithium-ion battery(LIB) with high Mn content faces the defects of high cost of neutralization and precipitation, poor economics of Mn extraction, and serious Li loss. Therefore, this paper introduces a comprehensive hydrometallurgical method for extracting valuable metals from high-Mn spent LIB. Particularly, directional precipitation of Mn was achieved by utilizing its redox properties, and shot-process extraction and enrichment of Li was realized by using the extractant HBL121. In a sulfuric acid system, control of the oxidant dosage to 0.8% resulted in high leaching efficiencies for Li, Ni, Co, and Mn, with values of 96.58%, 96.13%, 95.22%, and 94.24%, respectively, under optimal conditions which were C(H2SO4) of 3.5 mol/L, V(H2O2) of 0.8% (v/v), L/S of 10:1, temperature of 60 °C, and time of 60 min. Subsequently, the addition of KMnO4 dosage (Kp/Kt) in a ratio of 1:1 resulted in the precipitation of 98.47% of Mn as MnO2, with Ni and Li precipitation efficiencies of 0.2% and 0.1%, respectively. Cascade extraction of Ni and Co was reached by using Cyanex272 extractant from the solution after Mn precipitation. At an organic-to-aqueous phase ratio (O/A) of 1:5, the Co extraction efficiency reached 98.68%, whereas the loss efficiency of Ni was 5.53%, and Li was less than 0.1%. Adjusting the O/A to 1:1 increased the Ni extraction efficiency to 89.99% and Li loss to 8.95%. Finally, the HBL121 extractant was utilized to extract Li from the Li-rich solution, achieving 95.08% extraction efficiency. The Li was stripped with 2 mol/L H2SO4 from the load organic phase, realizing a Li concentration of 11.44 g/L. Thus, this process facilitates the comprehensive and efficient recovery of valuable metals such as Li, Ni, Co, and Mn from spent high-Mn LIB. Full article
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11 pages, 1830 KB  
Article
Material and Energy Flow Analysis of Hydrometallurgical Recycling for Lithium-Ion Battery Based on Aspen Plus
by Yifei Zhang, Valentin Mussehl and Dequan Piao
Coatings 2025, 15(9), 990; https://doi.org/10.3390/coatings15090990 - 26 Aug 2025
Viewed by 942
Abstract
The exponential growth of global electric vehicle deployment has precipitated a critical need for the sustainable recycling of end-of-life lithium-ion batteries (LIBs), particularly nickel–cobalt–manganese (NCM) ternary cathodes, which dominate the retired battery stream. This study establishes an integrated Aspen Plus-based hydrometallurgical process model, [...] Read more.
The exponential growth of global electric vehicle deployment has precipitated a critical need for the sustainable recycling of end-of-life lithium-ion batteries (LIBs), particularly nickel–cobalt–manganese (NCM) ternary cathodes, which dominate the retired battery stream. This study establishes an integrated Aspen Plus-based hydrometallurgical process model, focusing on “acid dissolution–LiOH precipitation–electrolysis” for closed-loop NCM recycling. Gibbs reactor-based dissolution kinetics is used for selective metal leaching (achieving > 99% efficiency at 185 kg/h acid flow), the thermodynamic prioritization of sequential hydroxide precipitation (Co → Ni → Mn at 10–60 kg/h LiOH), and the electrochemical regeneration of LiOH/H2SO4 from Li2SO4 (70.01 kg/h LiOH at 0.8 conversion). Material balance analysis confirms a net production of 10.01 kg LiOH per 100 kg of NCM feedstock with 41.87 kg of acid consumption, while the energy of electrolysis power is 452.96 kW at 6 V/1360 A/m2. This work provides a techno-economic framework for industrial-scale battery recycling. Full article
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12 pages, 3228 KB  
Communication
Green and Efficient Lithium Extraction from Spent NCM Batteries via Electromagnetic Radiation
by Ling Tong, Gui-Rong Zhang, Da-Shuai Li, Xing-Yu Huang, Yuan-Long Liu and Yan-Qing Cheng
Materials 2025, 18(17), 3975; https://doi.org/10.3390/ma18173975 - 25 Aug 2025
Viewed by 647
Abstract
The conventional recycling of spent lithium-ion batteries (LIBs) is hindered by high energy consumption and severe environmental pollution. In this study, a novel method utilizing high-frequency electromagnetic radiation was proposed to process the black mass derived from spent NCM-LIBs, significantly reducing both energy [...] Read more.
The conventional recycling of spent lithium-ion batteries (LIBs) is hindered by high energy consumption and severe environmental pollution. In this study, a novel method utilizing high-frequency electromagnetic radiation was proposed to process the black mass derived from spent NCM-LIBs, significantly reducing both energy consumption and chemical reagent usage. Conductive carbon black was introduced as an electromagnetic-wave-absorbing additive to improve the electromagnetic energy into thermal energy conversion efficiency during electromagnetic radiation. As a result, the decomposition and reduction of NCM materials can be completed within just 10 min at a microwave power of 500 W. Following electromagnetic irradiation, lithium was efficiently extracted via simple water leaching, achieving an extraction efficiency of 88.24%. Furthermore, a microwave heating device based on traveling-wave propagation was developed. Unlike conventional small-scale microwave systems that employ resonant cavities, this design enables improved heating uniformity, higher efficiency, and greater scalability for industrial microwave-assisted chemical processes. Full article
(This article belongs to the Special Issue Recycling and Electrode Materials of Lithium Batteries)
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28 pages, 4385 KB  
Review
Sustainable Recycling of Lithium-Ion Battery Cathodes: Life Cycle Assessment, Technologies, and Economic Insights
by Dongjie Pang, Haoyu Wang, Yimin Zeng, Xue Han and Ying Zheng
Nanomaterials 2025, 15(16), 1283; https://doi.org/10.3390/nano15161283 - 20 Aug 2025
Viewed by 1464
Abstract
Rapid growth of electric vehicles has increased demand for lithium-ion batteries (LIBs), raising concerns regarding their end-of-life management. This study comprehensively evaluates the closed-loop recycling of cathode materials from spent LIBs by integrating life cycle assessment (LCA), technoeconomic analysis, and technological comparison. Typical [...] Read more.
Rapid growth of electric vehicles has increased demand for lithium-ion batteries (LIBs), raising concerns regarding their end-of-life management. This study comprehensively evaluates the closed-loop recycling of cathode materials from spent LIBs by integrating life cycle assessment (LCA), technoeconomic analysis, and technological comparison. Typical approaches—including pyrometallurgy, hydrometallurgy, and other processes such as organic acid leaching and in situ reduction roasting—are systematically reviewed. While pyrometallurgy offers scalability, it is hindered by high energy consumption and excessive greenhouse gas emissions. Hydrometallurgy achieves higher metal recovery rates with better environmental performance but requires complex chemical and wastewater management. Emerging methods and regeneration techniques such as co-precipitation and sol–gel synthesis demonstrate potential for high-purity material recovery and circular manufacturing. LCA results confirm that recycling significantly reduces GHG emissions, especially for high-nickel cathode chemistry. However, the environmental benefits are affected by upstream factors such as collection, disassembly, and logistics. Technoeconomic simulations show that profitability is strongly influenced by battery composition, regional cost structures, and collection rates. The study highlights the necessity of harmonized LCA boundaries, process optimization, and supportive policy frameworks to scale environmentally and economically sustainable LIB recycling, ensuring long-term supply security for critical battery materials. Full article
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21 pages, 3739 KB  
Article
Occurrence State and Extraction of Lithium from Jinyinshan Clay-Type Lithium Deposit, Southern Hubei: Novel Blank Roasting–Acid Leaching Processes
by Hao Zhang, Peng Li, Wensheng Zhang, Jiankang Li, Zhenyu Chen, Jin Yin, Yong Fang, Shuang Liu, Jian Kang and Dan Zhu
Appl. Sci. 2025, 15(16), 9100; https://doi.org/10.3390/app15169100 - 18 Aug 2025
Viewed by 534
Abstract
Addressing the technological bottlenecks in the efficient utilization of clay-type Li deposits in China, this study systematically investigates Li occurrence states and develops clean extraction processes using the Jinyinshan clay-type Li deposit in southern Hubei as a case study. The research aims to [...] Read more.
Addressing the technological bottlenecks in the efficient utilization of clay-type Li deposits in China, this study systematically investigates Li occurrence states and develops clean extraction processes using the Jinyinshan clay-type Li deposit in southern Hubei as a case study. The research aims to provide technical guidance for subsequent geological exploration and development of such deposits. Analytical techniques, including AMICS, EPMA, and LA-ICP-MS, reveal that Li primarily occurs in structurally bound forms within cookeite (82.55% of total Li), illite (6.65%), and rectorite (5.20%), with mineral particle sizes concentrated in fine-grained fractions (<45 μm). Leveraging process mineralogical insights, two industrially adaptable blank roasting–acid leaching processes were innovatively developed. Process I employs a full flow of blank roasting–hydrochloric acid leaching–Li-Al separation–Ca/Mg removal–concentration for Li precipitation–three-stage counter-current washing. Optimizing roasting temperature (600 °C), hydrochloric acid concentration (18 wt%), and leaching parameters achieved a 92.37% Li leaching rate. Multi-step purification yielded lithium carbonate with >99% Li2CO3 purity and an overall Li recovery of 73.89%. Process II follows blank roasting–sulfuric acid leaching–Al removal via alum precipitation–Al/Fe removal–freeze crystallization for sodium sulfate removal–Ca/Mg removal–concentration for Li precipitation–three-stage counter-current washing. Parameter optimization and freezing impurity removal achieved an 89.11% Li leaching rate, producing lithium carbonate with >98.85% Li2CO3 content alongside by-products like crude sodium chloride and ammonium alum. Both processes enable resource utilization of Al-rich residues, with the hydrochloric acid-based method excelling in stability and the sulfuric acid-based approach offering superior by-product valorization potential. This low-energy, high-yield clean extraction system provides critical theoretical and technical foundations for scaling clay-type Li deposit utilization, advancing green Li extraction and industrial chain development. Full article
(This article belongs to the Special Issue Recent Advances in Geochemistry)
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18 pages, 2688 KB  
Article
Eco-Friendly Leaching of Spent Lithium-Ion Battery Black Mass Using a Ternary Deep Eutectic Solvent System Based on Choline Chloride, Glycolic Acid, and Ascorbic Acid
by Furkan Nazlı, Işıl Hasdemir, Emircan Uysal, Halide Nur Dursun, Utku Orçun Gezici, Duygu Yesiltepe Özçelik, Fırat Burat and Sebahattin Gürmen
Minerals 2025, 15(8), 782; https://doi.org/10.3390/min15080782 - 25 Jul 2025
Viewed by 1143
Abstract
Lithium-ion batteries (LiBs) are utilized in numerous applications due to advancements in technology, and the recovery of end-of-life (EoL) LiBs is imperative for environmental and economic reasons. Pyrometallurgical and hydrometallurgical methods have been used in the recovery of metals such as Li, Co, [...] Read more.
Lithium-ion batteries (LiBs) are utilized in numerous applications due to advancements in technology, and the recovery of end-of-life (EoL) LiBs is imperative for environmental and economic reasons. Pyrometallurgical and hydrometallurgical methods have been used in the recovery of metals such as Li, Co, and Ni in the EoL LiBs. Hydrometallurgical methods, which have been demonstrated to exhibit higher recovery efficiency and reduced energy consumption, have garnered increased attention in recent research. Inorganic acids, including HCl, HNO3, and H2SO4, as well as organic acids such as acetic acid and citric acid, are employed in the hydrometallurgical recovery of these metals. It is imperative to acknowledge the environmental hazards posed by these acids. Consequently, solvometallurgical processes, which involve the use of organic solvents with minimal or no water, are gaining increasing attention as alternative or complementary techniques to conventional hydrometallurgical processes. In the context of solvent systems that have been examined for a range of solvometallurgical methods, deep eutectic solvents (DESs) have garnered particular interest due to their low toxicity, biodegradable nature, tunable properties, and efficient metal recovery potential. In this study, the leaching process of black mass containing graphite, LCO, NMC, and LMO was carried out in a short time using the ternary DES system. The ternary DES system consists of choline chloride (ChCl), glycolic acid (GLY), and ascorbic acid (AA). As a result of the leaching process of cathode powders in the black mass without any pre-enrichment process, Li, Co, Ni, and Mn elements passed into solution with an efficiency of over 95% at 60 °C and within 1 h. Moreover, the kinetics of the leaching process was investigated, and Density Functional Theory (DFT) calculations were used to explain the leaching mechanism. Full article
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17 pages, 5410 KB  
Article
Mineral Phase Transformation and Leaching Behavior During the Roasting–Acid–Leaching Process of Clay-Type Lithium Ore in the Qaidam Basin
by Xiaoou Zhang, Jing Zhao, Yan Li, Dong An, Huaigang Cheng, Yuliang Ma and Huiping Song
Minerals 2025, 15(8), 777; https://doi.org/10.3390/min15080777 - 24 Jul 2025
Viewed by 420
Abstract
To address lithium extraction from clay-type lithium ore from the Qaidam Basin, this study identified key controlling factors through particle fractionation, acid-leaching–roasting experiments, and mineral characterization. The results demonstrate that particle size optimization enriched the lithium to 87.65 ppm, where a 74% leaching [...] Read more.
To address lithium extraction from clay-type lithium ore from the Qaidam Basin, this study identified key controlling factors through particle fractionation, acid-leaching–roasting experiments, and mineral characterization. The results demonstrate that particle size optimization enriched the lithium to 87.65 ppm, where a 74% leaching rate was achieved with 65 ppm extraction, which established intermediate-sized samples as optimal. During acid leaching, adsorbed lithium ions with a phyllosilicate interlayer were released via the ion exchange process instead of mineral dissolution, as verified by the Li-O/S-O peak shifts in the FTIR spectra. The roasting induced hydroxyl elimination, carbonate decomposition, and silicate restructuring but triggered lithium encapsulation via mineral phase reorganization, which caused a sharp leaching rate decline. Effective lithium extraction requires integrated particle size screening, acid-leaching optimization, and roasting-induced phase encapsulation disruption. This study established theoretical foundations for clay-type lithium ore exploitation. Full article
(This article belongs to the Section Mineral Processing and Extractive Metallurgy)
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21 pages, 3984 KB  
Article
Organic Acid Leaching of Black Mass with an LFP and NMC Mixed Chemistry
by Marc Simon Henderson, Chau Chun Beh, Elsayed Oraby and Jacques Eksteen
Recycling 2025, 10(4), 145; https://doi.org/10.3390/recycling10040145 - 21 Jul 2025
Viewed by 1239
Abstract
There is an increasing demand for the development of efficient and sustainable battery recycling processes. Currently, many recycling processes rely on toxic inorganic acids to recover materials from high-value battery chemistries such as lithium nickel manganese cobalt oxides (NMCs) and lithium cobalt oxide [...] Read more.
There is an increasing demand for the development of efficient and sustainable battery recycling processes. Currently, many recycling processes rely on toxic inorganic acids to recover materials from high-value battery chemistries such as lithium nickel manganese cobalt oxides (NMCs) and lithium cobalt oxide (LCOs). However, as cell manufacturers seek more cost-effective battery chemistries, the value of the spent battery value chain is increasingly diluted by chemistries such as lithium iron phosphate (LFPs). These cheaper alternatives present a difficulty when recycling, as current recycling processes are geared towards dealing with high-value chemistries; thus, the current processes become less economical. To date, much research is focused on treating a single battery chemistry; however, often, the feed material entering a battery recycling facility is contaminated with other battery chemistries, e.g., LFP feed contaminated with NMC, LCO, or LMOs. This research aims to selectively leach various battery chemistries out of a mixed feed material with the aid of a green organic acid, namely oxalic acid. When operating at the optimal conditions (2% solids, 0.25 M oxalic acid, natural pH around 1.15, 25 °C, 60 min), this research has proven that oxalic acid can be used to selectively dissolve 95.58% and 93.57% of Li and P, respectively, from a mixed LFP-NMC mixed feed, all while only extracting 12.83% of Fe and 8.43% of Mn, with no Co and Ni being detected in solution. Along with the high degree of selectivity, this research has also demonstrated, through varying the pH, that the selectivity of the leaching system can be altered. It was determined that at pH 0.5 the system dissolved both the NMC and LFP chemistries; at a pH of 1.15, the LFP chemistry (Li and P) was selectively targeted. Finally, at a pH of 4, the NMC chemistry (Ni, Co and Mn) was selectively dissolved. Full article
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12 pages, 23410 KB  
Article
Recycling and Separation of Valuable Metals from Spent Cathode Sheets by Single-Step Electrochemical Strategy
by Neng Wei, Yaqun He, Guangwen Zhang, Jiahao Li and Fengbin Zhang
Separations 2025, 12(7), 178; https://doi.org/10.3390/separations12070178 - 5 Jul 2025
Viewed by 473
Abstract
The conventional spent lithium-ion batteries (LIBs) recycling method suffers from complex processes and excessive chemical consumption. Hence, this study proposes an electrochemical strategy for achieving reductant-free leaching of high-valence transition metals and efficient separation of valuable components from spent cathode sheets (CSs). An [...] Read more.
The conventional spent lithium-ion batteries (LIBs) recycling method suffers from complex processes and excessive chemical consumption. Hence, this study proposes an electrochemical strategy for achieving reductant-free leaching of high-valence transition metals and efficient separation of valuable components from spent cathode sheets (CSs). An innovatively designed sandwich-structured electrochemical reactor achieved efficient reductive dissolution of cathode materials (CMs) while maintaining the structural integrity of aluminum (Al) foils in a dilute sulfuric acid system. Optimized current enabled leaching efficiencies exceeding 93% for lithium (Li), cobalt (Co), manganese (Mn), and nickel (Ni), with 88% metallic Al foil recovery via cathodic protection. Multi-scale characterization systematically elucidated metal valence evolution and interfacial reaction mechanisms, validating the technology’s tripartite innovation: simultaneous high metal extraction efficiency, high value-added Al foil recovery, and organic removal through single-step electrochemical treatment. The process synergized the dissolution of CM particles and hydrogen bubble-induced physical liberation to achieve clean separation of polyvinylidene difluoride (PVDF) and carbon black (CB) layers from Al foil substrates. This method eliminates crushing pretreatment, high-temperature reduction, and any other reductant consumption, establishing an environmentally friendly and efficient method of comprehensive recycling of battery materials. Full article
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