Search Results (241)

Leaching carbon residue (LCR) is a carbonaceous solid waste generated during the hydrometallurgical recycling of spent lithium-ion batteries. Although its high graphite content offers substantial potential for resource recovery, the residual heavy metals and fluorides present in LCR pose considerable environmental risks. Currently, LCR has not garnered sufficient attention within the industry, and the lack of recycling technologies suitable for large-scale disposal results in resource wastage and environmental pollution. To address these challenges, this study proposes an innovative strategy based on the concept of multi-field synergistic enhancement. The proposed approach involves recovering and regenerating graphite (RG) from LCR via low-temperature molten salt roasting assisted by high-pressure and mechanical activation. A combination of advanced characterization techniques was employed to compare the physicochemical properties of RG and commercial graphite (CG) and to systematically evaluate the technical feasibility of using regenerated graphite as an anode material for lithium-ion batteries. The results demonstrate that, under optimized molten salt roasting and aqueous leaching conditions, the carbon content of RG reaches 99.94 wt%, indicating the efficient removal of non-carbon impurities from the graphite matrix. Compared to CG, RG retains a typical layered structure; however, a lower carbon content (99.94 wt%) and poorer structural order (I_D/I_G = 0.30) are observed. In terms of electrochemical performance, RG delivers a discharge specific capacity of 394.64 mAh/g during the first cycle and exhibits excellent cycling stability, with a capacity retention of 86.50% after 100 cycles. This electrochemical performance is comparable to that of commercial graphite. The proposed multi-field-assisted low-temperature molten salt roasting technique enables the efficient recovery of high-value graphite resources from LCR, establishing a full-lifecycle recycling strategy tailored for lithium-ion battery applications. Full article

In this study, lithium was recovered from LiFePO₄ (LFP) cathode active materials through a two-step thermal process combining hydrogen reduction and chlorination roasting. Hydrogen reduction was conducted while varying temperature and holding time to promote oxygen removal from LFP and induce phase separation into Li₃PO₄ and iron phosphides (FeP and Fe₂P). Based on stoichiometric assessment using the degree of LFP decomposition and the reduction in oxygen moles, the optimal hydrogen-reduction condition was determined to be 900 °C for 1 h. Subsequently, CaCl₂ was selected as an appropriate chlorination agent using thermodynamic considerations, and the hydrogen-reduced product was reacted with CaCl₂ to convert Li₃PO₄ into water-soluble LiCl. The mass of LiCl produced was quantified as a function of reaction temperature. Water leaching enabled the separation of LiCl from the insoluble residues, resulting in an overall lithium recovery of 71.7%. Full article

Deep brines represent important sources of strategic resources such as lithium and potassium, characterized by low exploration costs and high utilization rates. The Triassic strata in the Sichuan Basin contain abundant lithium- and potassium-rich brines, and understanding their origin is essential for exploring similar deposits. This study integrated field sampling and published data to systematically analyze the brines through hydrochemical testing, statistical methods, and water–rock reaction experiments, providing a comprehensive genetic interpretation based on hydrochemical features, element correlations, and characteristic coefficients. The results indicated that the brines are of the Cl–Na type, and both the sodium–chloride and chloride–bromide coefficients are consistent with a marine origin. Evapo-concentration was identified as the main controlling factor for ion enrichment, with subordinate influence from atmospheric precipitation. The common source of Ca²⁺ and Mg²⁺ likely includes the widespread marine carbonate rocks and/or the alteration of Ca–Mg-bearing silicate minerals (e.g., in green bean rocks or detrital layers) during brine–rock interaction. The desulfation coefficient indicated that lithium enrichment depends on a closed reducing environment, while potassium enrichment shows minimal correlation with brine confinement. Leaching experiments confirmed that green bean rocks serve as a key effective source rock for lithium and potassium, with elemental leaching efficiency positively correlated with fluid salinity. Based on these findings, a “dual-recharge” genetic model is proposed: paleo-marine brines undergoing deep circulation and meteoric water infiltrating along tectonic fractures collectively leached lithium and potassium from the green bean rocks, providing abundant lithium and potassium to the deep brines. This study refines the metallogenic mechanism of lithium- and potassium-rich brines in the Triassic Sichuan Basin and provides guidance for regional brine mineral exploration. Full article

The strong adhesion between cathode materials and aluminium (Al) foil substrates presents a significant challenge in the recycling of spent lithium-ion batteries (LiBs). Conventionally, high temperatures and high concentrations of costly organic solvents such as N-methyl-2-pyrrolidone (NMP), dimethylacetamide (DMAC), dimethylformamide (DMF), and dimethyl sulfoxide (DMSO) are used to enhance ultrasonication-based delamination. In this study, a novel, eco-efficient approach was demonstrated for delaminating cathode materials from Al foil using a low-concentration organic citric-acid-assisted low-power ultrasonic treatment coupled with a gentle, low-power-per-volume mechanical mixing system at room temperature. The separation mechanism was attributed to the structure disruption, possibly swelling, of the polyvinylidene fluoride (PVDF) binder using low-concentration citric acid and the cavitation effects induced by ultrasound. Key parameters influencing the delamination efficiency included the solvent type, temperature, ultrasonic power, and treatment duration. Under optimised conditions, citric acid was used as the sonication reagent, with a process temperature of 20 °C, 60 W ultrasonic power, and 80 min of ultrasonication; a delamination efficiency of approximately 92% was achieved. The recovered cathode materials exhibited low agglomeration, favouring subsequent leaching processes. This work proposes an environmentally friendly and effective method for cathode and Al foil recovery from spent LiBs, integrating manual dismantling, ultrasonic treatment, and material separation. Full article

Amid growing environmental pressure and increasing demand for resource sustainability, the efficient recovery of valuable metals from spent lithium-ion batteries (LIBs) has become a critical challenge in the field of resource recycling. Therefore, a novel approach is presented for selective lithium (Li) and manganese (Mn) separation from LiNi_xCo_yMn_1−x−yO₂ by combining carbothermic reduction roasting and selective leaching. Low-cost glucose (C₆H₁₂O₆) was selected as the reduction roasting reductant, which converts the cathode materials into water-soluble lithium carbonate (Li₂CO₃), water-insoluble cobalt (Co), nickel (Ni), and manganese oxide (MnO). Wet magnetic separation was employed to preferentially extract Li while simultaneously removing excess carbon from Ni, Co, and MnO. Under optimal roasting conditions at 600 °C for 90 min followed by wet magnetic separation with a liquid–solid ratio of 30 mL/g for 30 min, 95.42% of Li was preferentially extracted. Subsequently, at a formic acid (HCOOH) concentration of 1.6 mol/L, liquid–solid ratio of 6 mL/g, and leaching time of 30 min, 94.29% of Mn was selectively extracted from the wet magnetic separation products, whereas Ni and Co were leached at 6.13% and 7.22%, respectively. The acid-leaching residue can be recycled as a Ni-Co alloy. Full article

Traditional lithium-ion battery recycling relies mainly on pyrolysis or chemical leaching to separate current collectors from electrode materials, inevitably resulting in secondary pollution. In contrast, eddy current separation (ECS) applied to crushed lithium-ion battery residues can substantially reduce the introduction of contaminants while minimizing material losses. However, the heterogeneous composition and diverse surface characteristics of crushed battery products, together with the conductivity degradation of electrode materials after long-term use, make conventional empirical particle–trajectory correlations inadequate for accurate optimization of ECS operating parameters. In addition, the coupling between process parameters and the resultant forces acting on conductive particles, as well as the associated separation trajectories, remain insufficiently understood, which severely limits process controllability. A force–trajectory model was therefore developed for spent current collectors and conductivity-degraded LiFePO₄ to describe their particle dynamics in an alternating magnetic field. The results demonstrate that the trajectory of LiFePO₄ is very similar to that of non-conductive materials, thereby facilitating its effective separation from metallic components in battery scrap. Eddy current separation experiments further confirm the accuracy of the model predictions with respect to separation trajectories and the influence of key process parameters. On this basis, optimization of the operating parameters increased the separation efficiency of the cathode material to above 95.1%. The clarified ECS mechanism for current collectors and electrode materials provides new insights into the mechanical pre-sorting and mechanistic understanding of lithium-ion battery fragments, thereby contributing to reductions in contaminant introduction during battery material recycling. Full article

The rapid increase in end-of-life lithium-ion batteries demands sustainable recycling routes for lithium recovery. This work presents a novel integrated hydrometallurgical–electrodialysis process designed specifically for recovering lithium from off-specification NMC cathode materials while enabling full reagent recyclability. Selective leaching with oxalic acid was optimised by setting the water-to-oxalic acid dihydrate ratio (H₂O/OA·2H₂O) to 7.3:1 w/w, achieving 81% lithium extraction at room temperature within 2 h while limiting the co-dissolution of Ni, Co and Mn to 0.2%, 1.6% and 1.7% by weight, respectively. The resulting leachate was processed in a four-chamber electrodialysis cell equipped with two Nafion 117 cation-exchange membranes and one Neosepta AMX-fmg anion-exchange membrane operating at −1.6 V versus Ag/AgCl, enabling 96% lithium recovery and 98% oxalic acid recovery. The regenerated oxalic acid stream (41.8 g L⁻¹) was fully restored to its initial concentration and reused in successive cycles without performance loss. Subsequent precipitation of lithium with Na₂CO₃ yielded 99.3%-pure Li₂CO₃. This combined leaching–electrodialysis–precipitation presents a high selectivity, low-waste, circular recovery system, offering a scientifically original approach that integrates reagent regeneration with high-purity lithium production. Full article

The electrochemical reuse of spent graphite from the negative electrodes of lithium-ion batteries is influenced by regeneration-induced changes in near-surface chemical and defect states. These states govern solid electrolyte interphase (SEI) re-formation, particularly when bulk contaminants are suppressed. Acidic malic-acid leaching and ethylenediaminetetraacetic acid chelation under alkaline conditions (pH 8.7) were compared under similar operating parameters to isolate the role of the leaching environment. This was followed by heat treatment at 1200 °C to decouple chemical cleaning from structural restoration. Both methods reduced the total impurities from 217.85 ppm to ~1.8 ppm, approaching that of commercial graphite. Despite the comparable bulk purity, depth-resolved X-ray photoelectron spectroscopy after formation cycling revealed distinct outermost surface states relevant to SEI re-formation: acidic processing yielded a more oxygenated carbon signature and higher LiOH fraction at the outermost surface (~16%), whereas alkaline chelation produced a more graphitic, carbonate-dominated surface with lower LiOH (~7%). Electrochemical and impedance measurements were consistent with these differences, suggesting that after the bulk impurities were minimized, resistance development was largely governed by the leaching-conditioned near-surface state, which biased the SEI composition. The comparison under matched conditions linked the regeneration environment to SEI-relevant surface speciation and provided a mechanistic basis for selecting regeneration routes to reuse spent graphite as a negative-electrode active material. Full article

The sustainable recycling of valuable metals from spent lithium-ion batteries (LIBs) is imperative for closing the resource loop. This study presents an integrated strategy for the stepwise recovery of metals from spent cathode sheets by in situ thermal reduction and selective leaching. The in situ thermal reduction converted the cathode material into a mixture of Li₂CO₃, LiAlO₂, Ni, Co, NiO, and CoO while simultaneously liberating the cathode materials from the Al current collector through binder removal. A combined process of water leaching, wet sieving, and filtration successfully achieved the separation and enrichment of Li-rich aqueous solution (near 60% Li), Al-rich coarse fraction (over 87% Al), and fine powder enriched with transition metals (over 90% of Ni, Co, and Mn). The pyrolysis gases released from binder decomposition were the key driver for forming Li₂CO₃, whereas the concurrent generation of LiF and LiAlO₂ limited direct water leaching efficiency. An alkaline leaching step was therefore introduced to co-extract Al and the associated Li from LiAlO₂, followed by an acid leaching step that recovered over 96% of the transition metals from the treated residue without external reductants. Complete mass balance analysis shows that the integrated process achieved overall recoveries of 91.86% for Li, 91.93% for Ni, 92.23% for Co, and 92.61% for Mn from all the combined leachate streams. Consequently, this work provides a reagent-saving, stepwise hydrometallurgical process for the comprehensive recycling of valuable metals from spent LIBs. Full article

The ability to precisely control the morphology of polylactide (PLA) microparticles is crucial for their biomedical applications, yet it is a challenge due to the interdependent nature of key parameters such as size, porosity, and surface topology. This study presents a systematic approach to fabricating PLA microparticles with tunable architecture via emulsion-solvent evaporation by investigating the interplay of polymer molecular weight (44–442 kDa), solution concentration (0.5–20% w/v), and porogen type (PEG, alkanes, lithium salts). We achieved precise size control from 5 to 500 μm, dictated by solution viscosity and the polymer’s crystallization tendency, with poly(L-lactide) yielding irregular particles and poly(D,L-lactide) forming perfect spheres. Furthermore, porogen selection was critical for porosity: alkanes enabled tailored pore networks, with longer chains (e.g., decane) producing larger pores via enhanced phase separation, whereas the double-emulsion method with Li₂CO₃ proved superior for macroporosity due to its slow leaching kinetics. This work provides a foundational guideline for the rational design of PLA microparticles with customized properties for targeted applications in drug delivery and tissue engineering. Full article

Conventional hydrometallurgical processes typically employ inorganic acids as leaching agents; however, these processes are frequently associated with significant environmental pollution and suffer from poor metal selectivity. Oxalic acid, as a green alternative leaching agent, demonstrates considerable application potential owing to its mild acidity, strong reducing capability, and superior complexing properties. This paper presents a systematic review of recent advances in the application of oxalic acid in hydrometallurgy, encompassing the coordination chemistry between oxalic acid and metal ions, its role as a selective leaching agent, and strategies for handling multicomponent oxalate-rich solutions. Furthermore, the industrial prospects of oxalic acid-based leaching technologies are discussed. Research indicates that oxalic acid exhibits high selectivity and efficient leaching performance for critical metals—including vanadium, lithium, cobalt, nickel, and gallium—from both primary ores and solid secondary resources. The underlying leaching mechanism primarily involves the formation of stable chelation complexes between oxalate anions and high charge-density metal ions, or valence state modulation via reduction, enabling selective dissolution and separation of target metals. In multicomponent oxalate systems, where metals predominantly exist as anionic complexes, established enrichment and purification approaches include anion exchange extraction, as well as precipitation techniques based on valence adjustment and double salt crystallization. To advance the industrial implementation of oxalic acid leaching technologies, further in-depth investigation is required into the recycling mechanisms of oxalic acid and the fundamental reaction pathways governing leaching and metal recovery processes. Full article

Mining activities generate vast quantities of waste each year, including mine tailings, bauxite residue, waste rock, and various metallurgical slags. Although these materials have traditionally been regarded as environmental liabilities, many possess physical and chemical properties that make them promising candidates for use in construction. This review synthesizes recent research on the utilization of major mining waste streams, with particular emphasis on pavement applications and other construction materials. The findings indicate that bauxite residue exhibits both pozzolanic and filler characteristics, demonstrating potential in asphalt mastics, asphalt mixtures, and other construction products. Nonetheless, its widespread adoption is constrained by issues such as high alkalinity, leaching risks, and concerns related to naturally occurring radioactivity. Mine tailings can be a substitute for fine aggregates and cement in a range of mixtures, though challenges, including pronounced material variability and environmental risks, persist. Waste rock offers favorable geotechnical properties for use in road bases and embankments, while metallurgical slags (e.g., copper, nickel, and lithium slags) provide functional pozzolanic activity and suitable aggregate qualities. Across all waste types, their incorporation into construction materials can conserve natural resources, reduce material costs, and support circular-economy and low-carbon development objectives. However, progress remains contingent upon advancements in material standards, pretreatment technologies, environmental protection measures, and large-scale field validation. Overall, this review underscores both the significant potential and the practical challenges associated with transforming mining waste into valuable and sustainable construction resources. Full article

Electronic waste (e-waste) is a growing solid waste stream with largely undisclosed and poorly characterized fluorinated constituents. We evaluated per- and polyfluoroalkyl substances (PFAS) leachability from four e-waste components (phone screens, phone plastics, capacitors, and Lithium-ion batteries) using a 30-day deionized water leaching test. PFAS were extracted by solid-phase extraction using weak anion exchange (WAX) cartridges and analyzed with a liquid chromatography triple-quadrupole mass spectrometer. In addition, the PFAS chemical profiles of e-waste components were characterized by non-targeted analysis. Leachable sums of detected PFAS (∑PFAS) were highest in phone screens (1739–1932 ng·kg⁻¹) and phone plastics (1575–2197 ng·kg⁻¹) and an order of magnitude lower in Lithium-ion batteries (148–158 ng·kg⁻¹) and capacitors (147–243 ng·kg⁻¹). Short-chain perfluoroalkyl acids (PFAAs) (e.g., PFBA, PFHxA) and legacy acids (e.g., PFOA, PFNA) were more prevalent in phone screens/plastics, whereas capacitors and batteries showed mixed sulfonate/carboxylate patterns (PFOS, PFHxS, and 6:2 FTS). Although capacitors and Lithium-ion batteries contained essential PFAS with high hazard potential at trace levels, phone screens and phone plastics pose a greater risk per mass due to higher ∑PFAS levels and larger volumes. Non-targeted analysis using Orbitrap Astral revealed CF₂/CF₂O homologous trends (confidence levels 2–3) with corroborating targeted findings. These findings highlight the need for PFAS-free alternatives, the disclosure of fluorinated additives, and stronger end-of-life management strategies to prevent PFAS releases from e-waste. Full article

In this work, a method for leaching black mass from spent Li batteries using oxalic acid was developed and experimentally verified with the objective of selectively separating lithium and cobalt. Oxalic acid proved to be an efficient and selective leaching agent. Under 1 M C₂H₂O₄, 120 min, L:S = 20, 80 °C and 300 rpm, a lithium yield of 90% was achieved, while cobalt dissolution remained low at 1.57%. Subsequently, cobalt spontaneously precipitated from the leachate within several hours, and the solid phase was fully separated after 24 h. The leachate contained minor amounts of accompanying metals, with dissolution yields of 0.5% Mn, 8% Fe and 1.4% Cu. These impurities were removed from the leachate by controlled pH adjustment using NaOH at ambient temperature and 450 rpm, with complete precipitation at pH 12. This procedure generated a purified lithium-rich leachate, which was converted into lithium oxalate by crystallisation at 105 °C. Subsequent calcination of the resulting solid at 450 °C for 30 min produced Li₂CO₃ with a purity of 91%. Based on the experimental findings, a conceptual technological process for selective lithium leaching using oxalic acid was proposed, demonstrating the potential of this method for sustainable lithium recovery. Full article

This study investigated the effect of mechanical activation on the physicochemical properties of lepidolite and the leaching behavior of mechanically activated samples in sulfuric acid (H₂SO₄). Lepidolite was mechanically activated using a high-energy planetary ball mill (PBM) at 400 RPM with a 20:1 ball-to-feed weight ratio (BFR, g:g) and the samples activated for different durations were characterized for amorphous phase content, particle size, and morphology using various solid analyses. X-ray diffraction (XRD) revealed the progressive amorphization of lepidolite, with the amorphous fraction increased from 34.1% (unactivated) to 81.4% after 60 min of mechanical activation. Scanning electron microscopy (SEM) showed that mechanically activated particles became fluffy and rounded, whereas unactivated particles retained lamellar and angular shapes. The reactivity of minerals after mechanical activation was evaluated through a 2 M H₂SO₄ leaching test at different leaching temperatures (25–80 °C) and time periods (30–180 min). Although the leaching efficiencies of Li and Al slightly improved at higher leaching temperatures and longer leaching times, the leaching of these metals was primarily governed by the mechanical activation time. The highest Li and Al leaching efficiencies—87.0% for Li and 79.4% for Al—were obtained from lepidolite that was mechanically activated for 60 min under leaching conditions of 80 °C and a 10% (w/v) solid/liquid (S/L) ratio for 30 min. The elemental mapping images of leaching feed and residue produced via energy dispersive spectroscopy (EDS) indicated that unactivated particles in the leaching residue had much higher metal content than mechanically activated particles. Kinetic analysis further suggested that leaching predominantly occurs at mechanically activated sites and the apparent activation energies calculated in this study (<3.1 kJ·mol⁻¹) indicate diffusion-controlled behavior with weak temperature dependence. This result confirmed that mechanical activation significantly improves reactivity and that the residual unleached fraction can be attributed to unactivated particles. Full article