• Resources Recycling
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• v.28 no.6
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• pp.79-86
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• 2019

Recently, the use of lithium ion battery(LIB) has increased. As a result, the price of lithium and the amount spent lithium on ion battery has increased. For this reason, research on recycling lithium in waste LIBs has been conducted1). In this study, the effect of roasting for the selective lithium leaching from the spent LIBs is studied. Chemical transformation is required for selective lithium leaching in NCM LiNi_xCo_yMn_zO₂) of the spent LIBs. The carbon in the waste EV cell powder reacts with the oxygen of the oxide at high temperature. After roasting at 550 ~ 850 ℃ in the Air/N₂ atmosphere, the chemical transformation is analysed by XRD. The heat treated powders are leached at a ratio of 1:10 in D.I water for ICP analysis. As a result of XRD analysis, Li₂CO₃ peak is observed at 700 ℃. After the heat treatment at 850 ℃, a peak of Li₂O was confirmed because Li₂CO₃ is decomposed into Li₂O and CO₂ over 723 ℃. The produced Li₂O reacted with Al at high temperature to form LiAlO₂, which does not leach in D.I water, leading to a decrease in lithium leaching ratio. As a result of lithium leaching in water after heat treatment, lithium leaching ratio was the highest after heat treatment at 700 ℃. After the solid-liquid separation, over 45 % of lithium leaching was confirmed by ICP analysis. After evaporation of the leached solution, peak of Li₂CO₃ was detected by XRD.

• Resources Recycling
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• v.28 no.5
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• pp.60-67
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• 2019

A valuable metal recovery from waste resources such as spent rechargeable secondary batteries is of critical issues because of a sharp increase in the amount of waste resources. In this context, it is necessary to research not only recycling waste lithium-ion batteries (LIBs), but also reusing valuable metals (e.g., Li, Co, Ni, Mn etc.) recovered from waste LIBs. In particular, the lithium hydroxide ($LiOH{\cdot}xH_2O$), which is of precursors that can be prepared by the recovery of Li in waste LIBs, can be reused as a catalyst, a carbon dioxide absorbent, and again as a precursor for cathode materials of LIB. However, most studies of recycling the waste LIBs have been focused on the preparation of lithium carbonate with a recovery of Li. Herein, we show the preparation of high purity lithium hydroxide powder along with the precipitation process, and the systematic study to find an optimum condition is also carried out. The lithium carbonate, which is recovered from waste LIBs, was used as starting materials for synthesis of lithium hydroxide. The optimum precipitation conditions for the preparation of LiOH were found as follows: based on stirring, reaction temperature $90^{\circ}C$, reaction time 3 hr, precursor ratio 1:1. To synthesize uniform and high purity lithium hydroxide, 2-step precipitation process was additionally performed, and consequently, high purity $LiOH{\cdot}xH_2O$ powder was obtained.

• Resources Recycling
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• v.28 no.5
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• pp.51-59
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• 2019

This study focused on the synthesis of the nickel hydroxide using ammonium sulfate in leaching solution from waste nickel-cadmium batteries. The effect of pH, temperature and the input amount of ammonium sulfate in leaching solution was investigated. The ammonium nickel sulfate with high purity was obtained in acidic leaching solution and the solution temperature of $60^{\circ}C$. The suitable molar ratio of the input amount of ammonium sulfate to nickel in solution is 2:1. The impurity about 1.4 at.% of Cd was included in the nickel hydroxide precipitates when ammonium nickel sulfate was used. At the process using sodium sulfide which precipitates the cadmium in solution, nickel and iron compounds were precipitated together.

• Proceedings of the KIPE Conference
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• 2018.07a
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• pp.225-227
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• 2018

일반적으로 리튬이온은 배터리들은 각 배터리마다 고유의 전기화학적 특성을 갖고 있으며 이러한 특성들로 인해서 직렬 또는 병렬로 패키징 되어서 팩으로 사용 될 때 각 셀 간의 전압 불균형이 발생하게 된다. 셀 벨런싱 회로 같은 셀 간 불균형을 회복시켜주는 기능이 없다면 배터리 팩 내의 셀 간 전압 불균형은 시간이 지남에 따라 더 커지게 되고 이는 배터리 팩의 노화를 가속 시키거나 배터리 팩의 성능을 저하시키는 원인이 된다. 이는 폐 리튬이온 배터리 팩을 재활용하는데 있어서도 반드시 고려해야하는 사항으로서 재활용 팩의 사용시간에 영향을 끼칠 수 있다. 위의 문제를 극복하기 위해서는 배터리 팩을 만들기 전에 스크리닝을 통해서 전기화학적 성분이 유사한 배터리들을 팩으로 만드는 것이 필요하다. 일반적으로 프레시 배터리의 용량은 거의 비슷하기 때문에 프레시 배터리 용량은 프레시 배터리를 스크리닝 하기 위한 많은 기준들 중에서 가중치가 크지 않지만 폐 리튬이온 배터리들은 각 배터리마다 고유의 전기화학적 특성을 갖을 뿐만 아니라 각 배터리마다 상이한 배터리 용량을 갖고 있기 때문에 각 배터리의 용량에 프레시 배터리를 스크리닝 할 때보다 큰 가중치를 두어 스크리닝 할 필요가 있다. 본 논문에서는 같은 전류 프로파일로 노화된 배터리 팩 내의 셀들의 전기화학적 특성을 분석하여 폐배터리 셀들을 재활용하기 위한 스크리닝 방법에 대해서 고찰한다.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.3
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• pp.91-106
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• 2019

The demand for lithium has increased sharply due to the explosive increase in lithium secondary batteries for environment-friendly vehicles (EV: Electric Vehicle, HEV: Hybrid Electric Vehicle, PHEV: Plug-in Hybrid Electric Vehicle). Traditionally, lithium has been produced mainly from lithium-containing minerals and brine, and recently it also has been recovered along with other valuable metals by recycling cathode materials of lithium secondary batteries. In this study, we comprehensively reviewed various recovering precesses of lithium from lithium-containing substances.

• Resources Recycling
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• v.30 no.6
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• pp.43-52
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• 2021

In this study, the optimal nitration process for selective lithium leaching from powder of a spent battery cell (LiNi_xCo_yMn_zO₂, LiCoO₂) was studied using Taguchi method. The nitration process is a method of selective lithium leaching that involves converting non-lithium nitric compounds into oxides via nitric acid leaching and roasting. The influence of pretreatment temperature, nitric acid concentration, amount of nitric acid, and roasting temperature were evaluated. The signal-to-noise ratio and analysis of variance of the results were determined using L₁₆(4⁴) orthogonal arrays. The findings indicated that the roasting temperature followed by the nitric acid concentration, pretreatment temperature, and amount of nitric acid used had the greatest impact on the lithium leaching ratio. Following detailed experiments, the optimal conditions were found to be 10 h of pretreatment at 700℃ with 2 ml/g of 10 M nitric acid leaching followed by 10 h of roasting at 275℃. Under these conditions, the overall recovery of lithium exceeded 80%. X-ray diffraction (XRD) analysis of the leaching residue in deionized water after roasting of lithium nitrate and other nitrate compounds was performed. This was done to determine the cause of rapid decrease in lithium leaching rate above a roasting temperature of 400℃. The results confirmed that lithium manganese oxide was formed from lithium nitrate and manganese nitrate at these temperatures, and that it did not leach in deionized water. XRD analysis was also used to confirm the recovery of pure LiNO₃ from the solution that was leached during the nitration process. This was carried out by evaporating and concentrating the leached solution through solid-liquid separation.

• Clean Technology
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• v.30 no.1
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• pp.28-36
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• 2024

As demand for electric vehicles increases, the market for lithium-ion batteries is also rapidly increasing. The battery life of lithium-ion batteries is limited, so waste lithium-ion batteries are inevitably generated. Accordingly, lithium was selectively preleached from waste lithium iron phosphate (LiFePO₄, hereafter referred to as the LFP) cathode material powder among lithium ion batteries, and iron phosphate (FePO₄) powder was recovered. The recovered iron phosphate powder was mixed with alkaline sodium carbonate (Na₂CO₃) powder and heat treated to confirm its crystalline phase. The heat treatment temperature was set as a variable, and then the leaching rate and powder characteristics of each ingredient were compared after water leaching using Di-water. In this study, lithium showed a leaching rate of approximately 100%, and in the case of powder heat-treated at 800 ℃, phosphorus was leached by approximately 99%, and the leaching residue was confirmed to be a single crystal phase of Fe₂O₃. Therefore, in this study, lithium, phosphorus, and iron components were individually separated and recovered from waste LFP powder.

• Environmental Engineering Research
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• v.25 no.1
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• pp.88-95
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• 2020

An investigation of rare metals recovery from LiNi_xCo_yMn_zO₂ cathode material of the end-of-life lithium-ion batteries is presented. To determine the influence of reductant on the leach process, the cathode material (containing Li 7.6%, Co 20.4%, Mn 19.4%, and Ni 19.3%) was leached in H₂SO₄ solutions either with or without H₂O₂. The optimal process parameters with respect to acid concentration, addition dosage of H₂O₂, temperature, and the leaching time were found to be 2.0 M H₂SO₄, 4 vol.% H₂O₂, 70℃, and 150 min, respectively. The yield of metal values in the leach liquor was > 99%. The leach liquor was subsequently treated by precipitation techniques to recover nickel as Ni(C₄H₇N₂O₂)₂ and lithium as Li₂CO₃ with stoichiometric ratios of 2:1 and 1.2:1 of dimethylglyoxime:Ni and Na₂CO₃:Li, respectively. Cobalt was recovered by solvent extraction following a 3-stage process using Na-Cyanex 272 at pH_eq ~5.0 with an organic-to-aqueous phase ratio (O/A) of 2/3. The loaded organic phase was stripped with 2.0 M H₂SO₄ at an O/A ratio of 8/1 to yield a solution of 114 g/L CoSO₄; finally recovered CoSO₄.xH₂O by crystallization. The process economics were analyzed and found to be viable with a margin of $476 per ton of the cathode material.

• Journal of the Korea Organic Resources Recycling Association
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• v.11 no.1
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• pp.102-112
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• 2003

The objective of this study was to investigate the effects of food waste and probiotics supplementation on productive performance and egg composition of laying hens. Total 120 layers (Brown Tetran) 22 weeks old were divided into five groups with 4 replicates for each treatments and raised in battery cage. The experimental design was completely randomized. The egg Production rate was significantly increased in layer supplemented with 0%, 0.5%, 1.0% and 1.5% of probiotic supplemented diets compared to control (P<0.05). At feeding with food waste and probiotic supplementation had no effect on the egg shell strength (P>0.05). Haugh unit of the eggs was significantly increased in layers fed with 1.5% of probiotic supplemented diet (P<0.05). The different levels of inclusion of the food waste and probiotic supplementation had not effect on egg shell color, blood spot and albumen index of the eggs (P<0.05). There were not significant differences in over all acceptability, juiciness, texture and color of the eggs from layer fed with different levels of wood waste and probiotic supplementation. The appearance and flavor significantly deteriorated in eggs from layers fed with probiotic diets compared to control (P<0.05).

• Resources Recycling
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• v.21 no.6
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• pp.58-64
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• 2012

A study on the solvent extraction for the separation and recovery of Ni and Li from the leaching solution of active cathode materials of Li-ion batteries was investigated using PC88A(2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester). The experimental parameters, such as the pH of the solution, concentration of extractant and phase ratio were observed. Experimental results showed that the extraction percent of Ni and Li and separation factor of Ni/Li were increased with increasing the equilibrium pH. More than 99.4% of Ni and 28.7% of Li were extracted in eq. pH 8.5 by 25% PC88A and the separation factor of Ni/Li was 411.6. From the analysis of McCabe-Thiele diagram, 99% of Ni was extracted by three extraction stages at phase ratio(A/O) of 1.5. Stripping of Ni and Li from the loaded organic phases can be accomplished by sulfuric acid as a stripping reagent and 50-60g/L of $H_2SO_4$ was effective for the stripping of Ni.