• Journal of the Korean Crystal Growth and Crystal Technology
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• v.30 no.2
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• pp.55-60
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• 2020

In the previous study, we reported the result to prepare lithium carbonate powder from various lithium-contained solution. Therefore, using the lithium hydroxide solution, it is conformed that the reaction could occur thermodynamically, and the recovery rate of lithium was 89.4 %. In this study, we carried out the experiment to prepare lithium carbonate powder through gas-liquid reactions with lithium hydroxide solution and CO₂ gas using ultrasound energy. In case ultrasonic energy is applied to the reaction of lithium carbonate, the recovery rate of lithium at room temperature was approximately 83.8 %, and the recovery rate of lithium was greatly increased to approximately 99.9 % at 60℃ reaction temperature. And when ultrasonic energy is not applied, the particle size of lithium carbonate powder was 7.7 ㎛ in D50. But the particle size of lithium carbonate powder was significantly reduced to 8.4 ㎛ in D50 under the influence of ultrasonic.

• Membrane Journal
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• v.34 no.3
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• pp.163-171
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• 2024

Growing demand on clean energy to control environmental pollution is growing rapidly. Rechargeable battery such as lithium ion battery is excellent source of clean energy but there is rapid depletion of lithium metal due to high demand and supply mismatch. Recovery of the precious metal from the battery waste is one of the possible solution along with the environmental pollution control. Membrane based separation method is highly successful commercial process available to recover lithium from the waste. This work will cover various methods reported recently and will be compiled in the form of a review.

• Resources Recycling
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• v.28 no.5
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• pp.3-18
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• 2019

Due to the increasing demand for clean energy, the consumption of lithium ion batteries (LIBs) is expected to grow steadily. Therefore, stable supply of lithium is becoming an important issue globally. Commercially, most of lithium is produced from the brine and minerals viz., spodumene, although various processes/technologies have been developed to recover lithium from other resources such as low grade ores, clays, seawaters and waste lithium ion batteries. In particular, commercialization of such recycling technologies for end-of-life LIBs being generated from various sources including mobile phones and electric vehicles(EVs), has a great potential. This review presents the commercial processes and also the emerging technologies for exploiting minerals and brines, besides that of newly developed lithium-recovery-processes for the waste LIBs. In addition, the future lithium-supply is discussed from the technical point of view. Amongst the emerging processes being developed for lithium recovery from low-grade ores, focus is mostly on the pyro-cum-hydrometallurgical based approaches, though only a few of such approaches have matured. Because of low recycling rate (<1%) of lithium globally compared to the consumption of lithium ion batteries (56% of lithium produced currently), processing of secondary resources could be foresighted as the grand opportunity. Considering the carbon economy, environment, and energy concerns, the hydrometallurgical process may potentially resolve the issue.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.5
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• pp.222-228
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• 2019

In this study, we carried out the experiment to prepare lithium carbonate powder through gas-liquid reactions with a lithium-containing solution and $CO_2$ gas using lithium hydroxide, lithium chloride, and lithium sulfate. Thermodynamically, the carbonation reaction of a lithium-containing solution showed that aqueous reaction of lithium hydroxide occurs spontaneously, but aqueous reactions of lithium chloride and lithium sulfate does not occur spontaneously. In the case of lithium hydroxide solution, the recovery rate of lithium carbonate was 69.8 % at room temperature ($25^{\circ}C$), and increased to 89.4 % at $60^{\circ}C$. In the case of lithium chloride and lithium sulfate solution, lithium carbonate could be prepared using sodium hydroxide as an additive, but the recovery rates were 19.2 % and 16.7 %, respectively.

• Resources Recycling
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• v.23 no.5
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• pp.21-27
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• 2014

A study on the solvent extraction for the recovery of Li from lithium-containing waste solution was investigated using $D_2EHPA$ as an extractant. The experimental parameters, such as the pH of the aqueous solution, concentration of extractant and phase ratio were observed. Experimental results showed that the extraction percentage of Li was increased with increasing the equilibrium pH. More than 50% of Li was extracted in eq. pH 6.0 by 20% $D_2EHPA$. From the analysis of McCabe-Thiele diagram, 95% of Li was extracted by four extraction stage at phase ratio(O/A) of 3.0. Stripping of Li from the loaded organic phases can be accomplished by sulfuric acid as a stripping reagent and 90 ~ 120 g/L of $H_2SO_4$ was effective for the stripping of Li. Finially, Li was concentrated about 11.85 g/L by continuous stripping process, and then lithium carbonate was prepared by precipitation method.

• Resources Recycling
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• v.22 no.4
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• pp.62-69
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• 2013

A study on the recovery of lithium and leaching behavior of NCM powder by carbon reduction for NCM-system Li-ion battery scraps was conducted. First of all, the oxide powders of NCM-system with layer structure were decomposed by carbon, lithium was converted to lithium carbonate by carbon reaction at above $600^{\circ}C$. The lithium carbonate powders with 99% purity were manufactured by washing method with water and concentration process for NCM powder after carbon reduction. The reaction yield was approximately 88% at $800^{\circ}C$ by carbon reduction. At this time, leaching efficiency at 2M sulfuric acid concentration was over 99% for cobalt, nickel and manganese.

• 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.32 no.3
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• pp.9-17
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• 2023

Efforts are currently underway to develop a method for efficiently recovering lithium from the cathode material of waste lithium iron phosphate batteries (LFP). The successful application of lithium battery recycling can address the regional ubiquity and price volatility of lithium resources, while also mitigating the environmental impact associated with both waste battery material and lithium production processes. The isomorphic substitution leaching process was used to recover lithium from spent lithium iron phosphate batteries. Lithium was leached by the isomorphic substitution of Fe²⁺ in LFP using a relatively inexpensive ferric chloride etching solution as a leaching agent. In the study, the leaching rate of lithium was compared using the ferric chloride etching solution at various multiples of the LFP molar ratio: 0.7, 1.0, 1.3, and 1.6 times. The highest lithium leaching rate was shown at about 98% when using 1.3 times the LFP molar ratio. Subsequently, to eliminate Fe, the leachate was treated with NaOH. The Fe-free solution was then used to synthesize lithium carbonate, and the harvested powder was characterized and validated. The surface shape and crystal phase were analyzed using SEM and XRD analysis, and impurities and purity were confirmed using ICP analysis.

• Resources Recycling
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• v.28 no.4
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• pp.30-36
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• 2019

In this study, Li powder was recovered from the by-product of LNO ($Li_2NiO_2$) process, which is the positive electrode active material of waste lithium ion battery, through the $CO_2$ thermal reaction process. In the process of recovering Li powder, the $CO_2$ injection amount is 300 cc/min. The $Li_2NiO_2$ award was phase-separated into the $Li_2CO_3$ phase and the NiO phase by holding at $600^{\circ}C$ for 1 min. After this, the collected sample:distilled water = 1:50 weight ratio, and after leaching, the solution was subjected to vacuum filtration to recover $Li_2CO_3$ from the solution, and the NiO powder was recovered. In order to increase the purity of Ni, it was maintained in $H_2$ atmosphere for 3 hours to reduce NiO to Ni. Through the above-mentioned steps, the purity of Li was 2290 ppm and the recovery was 92.74% from the solution, and Ni was finally produced 90.1% purity, 92.6% recovery.

• Resources Recycling
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• v.22 no.3
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• pp.43-49
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• 2013

A study on the recovery of lithium and leaching behavior of NCM powder by hydrogen reduction for NCM system Li-ion battery scraps was investigated. The reductive rate was about 93% at $800^{\circ}C$ by hydrogen treatment. The lithium carbonate with 99% purity was manufactured by using $CO_2$ gas and washing method with water for NCM powder after hydrogen reduction. As a result of comparing the powders before and after the hydrogen reduction treatment for acid leaching behavior we obtained 32% enhanced leaching rate of cobalt, 45% enhanced leaching rate of nickel and the 90% leaching effect for manganese by hydrogen reduction at 2M $H_2SO_4$ concentration condition.