| 1. |
- Balachandran, Srija, et al.
(författare)
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Comparative study for selective lithium recovery via chemical transformations during incineration and dynamic pyrolysis of EV li-ion batteries
- 2021
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Ingår i: Metals. - : MDPI AG. - 2075-4701. ; 11:8
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Tidskriftsartikel (refereegranskat)abstract
- Selective leaching of Li from spent LIBs thermally pretreated by pyrolysis and incineration between 400 and 700 °C for 30, 60, and 90 min followed by water leaching at high temperature and high L/S ratio was examined. During the thermal pretreatment Li2CO3 and LiF were leached. Along with Li salts, AlF3 was also found to be leached with an efficiency not higher than 3.5%. The time of thermal pretreatment did not have a significant effect on Li leaching efficiency. The leaching efficiency of Li was higher with a higher L/S ratio. At a higher leaching temperature (80 °C), the leaching of Li was higher due to an increase in the solubility of present Li salts. The highest Li leaching efficiency of nearly 60% was observed from the sample pyrolyzed at 700 °C for 60 min under the leaching condition L/S ratio of 20:1 mL g−1 at 80 °C for 3 h. Furthermore, the use of an excess of 10% of carbon in a form of graphite during the thermal treatment did not improve the leaching efficiency of Li.
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| 2. |
- Ottink, Thomas, 1996, et al.
(författare)
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Novel approach to recycling of steel swarf using hydrometallurgy
- 2022
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Ingår i: Resources, Conservation and Recycling. - : Elsevier BV. - 0921-3449 .- 1879-0658. ; 185
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Tidskriftsartikel (refereegranskat)abstract
- Steel swarf is a hazardous waste which is challenging to recycle due to its high content of heavy metals and cutting fluids and is today commonly landfilled. The swarf can contain up to 80% iron and represents a potential secondary raw material for production of reagents like ferric chloride, which can be utilized in wastewater treatment. This work presents a novel hydrometallurgical approach for recycling steel swarf and production of ferric chloride by selective separation of iron from heavy metals. Swarf containing 69% iron was leached with hydrochloric acid. A leachate containing 24.600 mg/L Fe with 150 mg/L Mn, 12 mg/L Ni and <1 mg/L Cr and Mo was obtained. The oil-based cutting fluids largely remained in the solid residue with only 1% dissolution in the aqueous phase. These findings showed that ferric chloride solutions of 99% purity can be produced from steel swarf in a single leaching step.
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| 3. |
- Petranikova, Martina, 1983, et al.
(författare)
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Recovery of critical metals from EV batteries via thermal treatment and leaching with sulphuric acid at ambient temperature
- 2022
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Ingår i: Waste Management. - : Elsevier BV. - 0956-053X .- 1879-2456. ; 140, s. 164-172
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Tidskriftsartikel (refereegranskat)abstract
- In the upcoming years, todaýs e-mobility will challenge the capacity of sustainable recycling. Due to the presence of organic components (electrolyte, separator, casings, etc.), future recycling technologies will combine thermal pre-treatment followed by hydrometallurgical processing. Despite the ongoing application of such treatment, there is still a lack of information on how applied parameters affect subsequent metal recovery. In this study, both oxidative and reductive conditions in dependence on temperature and time were studied. Qualitative and quantitative characterizations of the samples after treatment were performed followed by leaching with 2 M sulphuric acid at ambient temperature to determine the leachability of valuable metals such as Co, Mn, Ni and Li. Moreover, the negative or positive effect of treatment on the leachability of the main impurities (Cu and Al) was determined. Since the presence of carbon affects the degree of active material reduction, it's content after each thermal treatment was determined as well. If all variables, temperature and time of thermal processing are taken into account, pyrolysis at 700 °C for 30 min is the optimal treatment. Under these conditions, full recovery is reached after 2 min for Li, 5 min for Mn and 10 min for both Co and Ni. In the case of the incineration, only processing at 400 and 500 °C promoted higher recovery of metals, while the treatment at 600 and 700 °C led to the formation of less leachable species.
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| 4. |
- Rouquette, Léa, 1995, et al.
(författare)
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Complete and selective recovery of lithium from EV lithium-ion batteries: Modeling and optimization using oxalic acid as a leaching agent
- 2023
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Ingår i: Separation and Purification Technology. - 1873-3794 .- 1383-5866. ; 320
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Tidskriftsartikel (refereegranskat)abstract
- The necessity of a feasible process for the recycling of lithium-ion batteries is nowadays evident due to the significant demand for raw materials for battery production, but also due to legislative requirements to achieve certain recycling efficiency with sufficient quality of the products. Special conditions to achieve high lithium recovery and its use in new batteries represent a challenge for a commercial hydrometallurgical approach. In this work, an early selective recovery of lithium using oxalic acid as a leaching agent is investigated. The different solubility of transition metals oxalates in comparison to lithium oxalate was the main driving force to achieve selective separation in the leaching step. Nickel, cobalt, and manganese oxalates are insoluble and remained in the solid residue, while lithium oxalate was dissolved in the solution. Using a design of experiments to optimize the operation, optimal parameters were identified as 60 °C, 60 min, 0.6 M oxalic acid, resulting in 98.8% leaching yield for lithium, while less than 0.5 % of cobalt and nickel, and 1.5% of manganese were leached. This can significantly improve the lithium recovery in the current recycling processes. Moreover, aluminum was completely dissolved, which is a phenomenon not reported previously. It would constitute an advantage to the subsequent recycling operations.
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| 5. |
- Rouquette, Léa, 1995, et al.
(författare)
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Intensification of lithium carbonation in the thermal treatment of spent EV Li-ion batteries via waste utilization and selective recovery by water leaching
- 2023
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Ingår i: Resources, Conservation and Recycling Advances. - : Elsevier BV. - 2667-3789. ; 17
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Tidskriftsartikel (refereegranskat)abstract
- The recycling of lithium-ion batteries remains an essential question, the recovery of lithium is a central matter since the European Commission identified it as a critical raw material. This article proposes a more effective technology in which lithium will be recovered as lithium carbonate earlier in the recycling process using thermal pre-treatment and water leaching. Two thermal treatments are compared: incineration and pyrolysis, the whole cell (cathode, anode, current collector foils, and separator) is thermally treated in a first route, while the separator is removed, in a second route. The separator's presence showed a significant positive effect on the recovery, with an optimal recovery of 62% after pyrolysis at 700°C for 1 h and water leaching at 25°C with a solid-liquid ratio of 1:50 g/ml. Under these conditions, the solution purity was 92%, and aluminum was leached together with lithium. After evaporation, lithium carbonate and fluoride are found in the residue.
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| 6. |
- Vieceli, Nathalia Cristine, 1989, et al.
(författare)
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Hydrometallurgical recycling of EV lithium-ion batteries: Effects of incineration on the leaching efficiency of metals using sulfuric acid
- 2021
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Ingår i: Waste Management. - : Elsevier BV. - 0956-053X .- 1879-2456. ; 125, s. 192-203
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Tidskriftsartikel (refereegranskat)abstract
- The growing demand for lithium-ion batteries will result in an increasing flow of spent batteries, which must be recycled to prevent environmental and health problems, while helping to mitigate the raw materials dependence and risks of shortage and promoting a circular economy. Combining pyrometallurgical and hydrometallurgical recycling approaches has been the focus of recent studies, since it can bring many advantages. In this work, the effects of incineration on the leaching efficiency of metals from EV LIBs were evaluated. The thermal process was applied as a pre-treatment for the electrode material, aiming for carbothermic reduction of the valuable metals by the graphite contained in the waste. Leaching efficiencies above 70% were obtained for Li, Mn, Ni and Co after 60 min of leaching even when using 0.5 M sulfuric acid, which can be linked to the formation of more easily leachable compounds during the incineration process. When the incineration temperature was increased (600–700 °C), the intensity of graphite signals decreased and other oxides were identified, possibly due to the increase in oxidative conditions. Higher leaching efficiencies of Mn, Ni, Co, and Li were reached at lower temperatures of incineration (400–500 °C) and at higher leaching times, which could be related to the partial carbothermic reduction of the metals.
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| 7. |
- Vieceli, Nathalia Cristine, 1989, et al.
(författare)
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Optimization of manganese recovery from a solution based on lithium-ion batteries by solvent extraction with d2ehpa
- 2021
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Ingår i: Metals. - : MDPI AG. - 2075-4701. ; 11:1, s. 1-20
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Tidskriftsartikel (refereegranskat)abstract
- Manganese is a critical metal for the steelmaking industry, and it is expected that its world demand will be increasingly affected by the growing market of lithium-ion batteries. In addition to the increasing importance of manganese, its recycling is mainly determined by trends in the recycling of iron and steel. The recovery of manganese by solvent extraction has been widely investigated; however, the interaction of different variables affecting the process is generally not assessed. In this study, the solvent extraction of manganese from a solution based on lithium-ion batteries was modeled and optimized using factorial designs of experiments and the response surface methodology. Under optimized conditions (O:A of 1.25:1, pH 3.25, and 0.5 M bis(2-ethylhexyl) phosphoric acid (D2EHPA)), extractions above 70% Mn were reached in a single extraction stage with a coextraction of less than 5% Co, which was mostly removed in two scrubbing stages. A stripping product containing around 23 g/L Mn and around 0.3 g/L Co can be obtained under optimized conditions (O:A of 8:1, 1 M H2SO4 and around 13 min of contact time) in one stripping stage.
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| 8. |
- Vieceli, Nathalia Cristine, 1989, et al.
(författare)
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Recycling of Li-Ion Batteries from Industrial Processing: Upscaled Hydrometallurgical Treatment and Recovery of High Purity Manganese by Solvent Extraction
- 2023
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Ingår i: Solvent Extraction and Ion Exchange. - : Informa UK Limited. - 0736-6299 .- 1532-2262. ; 41:2, s. 205-220
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Tidskriftsartikel (refereegranskat)abstract
- Manganese plays a central role in lithium-ion batteries (LIBs) but its recycling is rarely addressed when compared to other valuable metals present in LIBs, such as Co and Ni. Thus, the main goal of this work was to study and achieve the separation of Mn from Co and Ni by solvent extraction from a leachate obtained from LIBs using hydrochloric acid in an upscaled reactor, which is an innovative aspect of this work. The results confirmed the high selectivity of D2EHPA towards Mn, which could be completely extracted in two stages (0.5 M D2EHPA at pH 2.5). The main co-extracted metals were Al, Cu and Co, but with lower concentrations than Mn. The behavior of minor impurities such as Zn and Mg was also monitored. Scrubbing using manganese chloride was crucial to remove impurities from the loaded organic and prevent their presence in the stripping product, and high O:A ratios negatively affected the scrubbing efficiency. Keeping the concentration of HCl up to 0.5 M in the stripping stage helped to limit the stripping of impurities. Manganese oxide was precipitated as a product with 99.5% purity (with traces of Zn, Cu and Co), which could be reused in the battery value chain.
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| 9. |
- Vieceli, Nathalia Cristine, 1989, et al.
(författare)
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Recycling of Lithium-Ion Batteries: Effect of Hydrogen Peroxide and a Dosing Method on the Leaching of LCO, NMC Oxides, and Industrial Black Mass
- 2023
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Ingår i: ACS Sustainable Chemistry & Engineering. - 2168-0485. ; 11:26, s. 9662-9673
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Tidskriftsartikel (refereegranskat)abstract
- The effect of hydrogen peroxide on the leachability ofdifferentreference cathode active materials used in lithium-ion batteries (LCO,NMC 111, NMC 622, and NMC 811) was investigated using 2 M H2SO4. An innovative method was used to monitor the consumptionand residual concentration of hydrogen peroxide, which can help optimizeits addition and improve the economy and resource yield of the process.The reducing effect of hydrogen peroxide was compared using two methodsof adding it. Leaching with hydrogen peroxide significantly improvedthe dissolution and 100% yield was reached within 15 min for the NMCoxides (except NMC 811) and within 30 min for LCO. Co and Ni weremore easily leached from NMC 811 compared to other NMC oxides. Thedissolution of metals from LCO was in general slower. Cu and Al canalso act as reducing agents and their presence increased the leachingyield of the transition metals, especially Mn, and resulted in lessresidual hydrogen peroxide. The H2O2 additionmethod (all at once or charged at multiple occasions) did not influencethe maximum leachability (except for Mn/NMC 811) or the amount ofconsumed hydrogen peroxide, but the rate of dissolution was slowerwhen charging at multiple times. The optimal conditions determinedfor the reference NMC 111 cathode material [3% v/v H2O2 (59% w/w), S/L 1:20 g/mL, 2 M H2SO4, 50 & DEG;C] were applied for an industrial black mass sample (Li(1.09)Ni(0.31)Mn0(.39)Co(0.39)O(2)). The result was 100% yield for Li, Mn, and Ni, after 15min and 100% yield for Co after 60 min. Optimizedprocess decreases reagents consumption and carbonfootprint and increases the efficiency of the recycling process.
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| 10. |
- Vieceli, Nathalia Cristine, 1989, et al.
(författare)
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Solvent extraction of cobalt from spent lithium-ion batteries: Dynamic optimization of the number of extraction stages using factorial design of experiments and response surface methodology
- 2023
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Ingår i: Separation and Purification Technology. - : Elsevier BV. - 1873-3794 .- 1383-5866. ; 307
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Tidskriftsartikel (refereegranskat)abstract
- The optimization of lithium-ion batteries (LiBs) recycling is crucial not only from a waste management perspective but also to decrease the dependence on imports of critical raw materials. In addition, the diversification of the recycling technologies is very important for better flexibility of the market. This study aims at investigating the recovery of Co from spent LiBs using solvent extraction from a real chloride-based solution obtained after the removal of Mn, which is very rarely reported. Cyanex 272 was used as the extractant and the effect of several variables on the extraction efficiency was considered to model and optimize the separation of Co and Ni. The number of extraction stages directly affects not only the process efficiency but also its cost. Thus, in this work, a novel approach was developed to assist in the selection of the number of extraction stages using a dynamic method based on the factorial design of experiments and response surface methodology combined with the Kremseŕs Equation. This method can assist the process design, decrease the overall cost of the operation, and optimize the separation of Co and Ni in a reduced number of extraction stages. The concentration of Co and Ni in the feed solutions is ∼ 8.3 g/L and 1.9 g/L, respectively. Based on the results, 98% extraction efficiency for Co can be achieved in 1 to 2 extraction stages with low co-extraction of Ni (<5%) when using 0.6–0.8 M Cyanex 272, O:A ratio below 1 and pH ∼ 5, but several combinations of conditions could provide similar results.
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