• Clean Technology
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• v.29 no.2
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• pp.87-94
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• 2023

The recovery of valuable metals from waste lithium-based secondary batteries is very important in terms of efficiently utilizing earth's limited number of resources. Currently, the cathode material of a LiFePO₄ battery, a type of battery which is widely used in automobiles, contains approximately 5% lithium. After use, the lithium in these batteries can be used again as a raw material for new batteries through lithium recycling. In this study, low-concentration sulfuric acid, a commonly used type of inorganic acid, was used to selectively leach the lithium contained in a waste LiFePO₄ cathode material powder. In addition, in order to compare and analyze the leaching efficiency and separation efficiency of each component, the optimalleaching conditions were derived by applying a two-step leaching process with pulp density being used as a variable during leaching. When leaching with pulp density as a variable, it was confirmed that at a pulp density of 200 g/L, the separation efficiency was approximately 200 times higher than at other pulp densities because the iron and phosphorus components were hardly leached at this pulp density. Accordingly, the pulp density of 200 g/L was used tooptimize the leaching conditions for the selective leaching and recovery of lithium.

• Membrane Journal
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• v.31 no.5
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• pp.315-326
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• 2021

Lithium ion battery (LIB) demands increase every year globally to reduce the burden on fossil fuels. LIBs are used in electric vehicles, stationary storage systems and various other applications. Lithium is available in seawater, salt lakes, and brines and its extraction using environmentally friendly and inexpensive methods will greatly relieve the pressure in lithium mining. Membrane separation processes, mainly nanofiltration (NF), is an effective way for the separation of lithium metal from solutions. Electrodialysis and electrolysis are other separation processes used for lithium separation. The process of reverse osmosis (RO) is already a well-established method for the desalination of seawater; therefore, modifying RO membranes to target lithium metals is an excellent alternative method in which the only bottleneck is the interfering presence of other metal elements in the solution. Selectively removing lithium by finding or developing suitable NF membranes can be challenging, but it is nonetheless an exciting area of research. This review discusses in detail about lithium recovery via nanofiltration, electrodialysis, electrolysis and other processes.

• Resources Recycling
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• v.31 no.4
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• pp.26-33
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• 2022

Owing to the demand for lithium-ion batteries, the recovery of valuable metals from waste lithium-ion batteries is required in future. A pyrometallurgical treatment is appropriate for recycling a large number of waste lithium-ion batteries, but Li loss to slag and dust present a significant challenge. This research investigated carbonation roasting and water leaching behaviors in Li-ion batteries by graphite addition to recover Li from the NCM-based cathode materials of waste Li-ion batteries. When 10 wt% of graphite was added, CO and CO₂ gases were emitted with a rapid weight reduction at apporoximately 850 K, when heated in Ar and CO₂ atmosphere. After the rapid weight reduction, NCM was decomposed and reduced to metal oxides and pure metals. In the carbonation roasting of black powder (NCM+graphite), O₂ is generated via the decomposition of NCM, and an oxides, such as Li₂O and NiO were were also generated. Subsequently, Li₂O reacts with CO₂ to generate Li₂CO₃, and a part of NiO was reduced by graphite to produce metal Ni. In addition, up to 94.5 % Li₂CO₃ with ~99.95 % purity was recovered via water leaching after carbonation roasting.

• Membrane Journal
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• v.32 no.6
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• pp.401-410
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• 2022

Demand for lithium hydroxide (LiOH) is annually increasing due to its efficiency and safety for the environment in comparison to its current alternatives. Lithium can be found in different salty and brine lakes which later synthesized to produce LiOH for various applications. Different methods are used to separate and recover lithium ions, the most common of which is electrodialysis (ED). ED is a membrane-based separation technique which works on potential difference of its layers as a driving force to push ions from one side to another. The ion exchange membrane (IEM) in ED makes the process efficient because of the perm selectivity of different ions vary depending on their hydrodynamic volume. In this review, the different alteration strategies of both ED and IEM, to enhance the recovery of lithium ions are discussed.

• Proceedings of the Korean Institute of Resources Recycling Conference
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• 2005.10a
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• pp.173-177
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• 2005

리튬이온 2차전지(Lithium ion battery, LIB)는 기존에 사용되던 전지에 비해 에너지 밀도가 높고 충방전 사이클이 우수하다. 이 때문에 휴대전화와 노트북 등에 수요가 급속하게 증가하고 있으며 1995년 LIB의 생산량은 4천만 개에서 2004년에는 약 8억 개로 20배 이상 증가하였다. 이에 따라 폐LIB도 급속하게 증가하게 되어 전국적인 재활용 시스템의 확보가 필요한 실정이다. 본 연구에서는 폐LIB에 함유되어 있는 유가금속 중에서 리튬코발트옥사이드(이하 $LiCoO_2$)를 회수하기 위하여 분쇄기(orient vertical cutting mill)와 진동 Screen을 사용하여 유기분리막, 금속류(Aluminium foil, Copper foil, case 등) 그리고 전극물질(lithium cobalt oxide와 graphite 등의 혼합 분말)로 분리하였다. 전극물질에서 $LiCoO_2$와 graphite 분리를 위한 전처리 단계로서 $500^{\circ}C$ 정도의 열처리를 하여 $LiCoO_2$의 표면 성질을 변화시켜 부유선별에 의해 $LiCoO_2$와 graphite의 분리가 가능하도록 하였다. 부유선별 실험 결과 93% 이상의 순도를 가지는 $LiCoO_2$를 92% 이상 회수할 수 있었다.

• Resources Recycling
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• v.30 no.1
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• pp.44-52
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• 2021

This study investigated the effect of the type of alkaline precipitant used on the synthesis of lithium hydroxide by examining the behavior of lithium hydroxide produced using lithium sulfate recovered from a waste lithium secondary battery as a raw material. The double-replacement reaction (DRR) process was used to remove the impurities contained in the lithium salt precursor of lithium sulfate and to improve the efficiency of the synthesis of lithium hydroxide. The experiment was conducted by control the molar ratio of the precursor ([Li]/[OH]), the reaction temperature, and the composition of the alkaline precipitant (KOH, Ca(OH)2, Ba(OH)2) used for the production of highly-crystalline lithium hydroxide. A secondary solid-liquid separation was performed following the reaction to remove the impurities generated, and the purified aqueous solution of lithium hydroxide was evaporated to remove the moisture and obtain the product as a powder. The crystallinity and synthesis behavior of the product were examined.

• Resources Recycling
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• v.32 no.1
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• pp.21-32
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• 2023

Because the application of lithium has gradually increased for the production of lithium ion batteries (LIBs), more research studies about recycling using solvent extraction (SX) should focus on Li⁺ recovery from the waste solution obtained after the removal of the valuable metals nickel, cobalt and manganese (NCM). The raffinate obtained after the removal of NCM metal contains lithium ions and other impurities such as Na ions. In this study, we optimized a selective SX system using di-(2-ethylhexyl) phosphoric acid (D2EHPA) as the extractant and tri-n-butyl phosphate (TBP) as a modifier in kerosene for the recovery of lithium from a waste solution containing lithium and a high concentration of sodium (Li⁺ = 0.5 ~ 1 wt%, Na⁺ = 3 ~6.5 wt%). The extraction of lithium was tested in different solvent compositions and the most effective extraction occurred in the solution composed of 20% D2EHPA + 20% TBP + and 60% kerosene. In this SX system with added NaOH for saponification, more than 95% lithium was selectively extracted in four extraction steps using an organic to aqueous ratio of 5:1 and an equilibrium pH of 4 ~ 4.5. Additionally, most of the Na⁺ (92% by weight) remained in the raffinate. The extracted lithium is stripped using 8 wt% HCl to yield pure lithium chloride with negligible Na content. The lithium chloride is subsequently treated with high purity ammonium bicarbonate to afford lithium carbonate powder. Finally the lithium carbonate is washed with an adequate amount of water to remove trace amounts of sodium resulting in highly pure lithium carbonate powder (purity > 99.2%).

• Resources Recycling
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• v.32 no.1
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• pp.13-20
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• 2023

The objective of this article is to summarize the commercial lithium ion battery (LIB) recycling processes in Korea and to suggest new direction for LIB recycling. A representative LIB recycler, SungEel Hitech Co. has successfully operated the LIB recycling process for over 10 years, and new recycling processes were recently proposed or developed by many recycling companies and battery manufacturers. In the new recycling processes, lithium is recovered before nickel and cobalt due to the rapid rise in lithium prices, and metal sulfate solution as final product of recycling process can be supplied to manufacturers. The main problem that the new recycling process will face is impurities, which will mainly come from end-of-life electric vehicles or new additives in LIB, although the conventional processes must be improved for mass processing.

• Journal of the Korean Chemical Society
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• v.63 no.6
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• pp.440-445
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• 2019

It has developed a method that can recover efficiently the reproducible resources from the vehicle waste lithium second battery module. Module cell consists of copper thin film, aluminum thin film and diaphragm made with polymer between these thin films. Cell was disassembled completely without any damage in glove box and through several steps. Preferentially, cathode active material was separated from aluminum thin film at heat treatment of 400 ℃. The retrieved cathode active material was then obtained as high purity after calcining at 800 ℃ to remove residual carbon. Based on this study, it was found that rare metals such as Co, Ni, Mn and Li made up of cathode active material could recover above 80% from aluminum thin film.

• Analytical Science and Technology
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• v.13 no.3
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• pp.309-314
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• 2000

The quantitative analysis of various trace metals including fission products in lithium molten salts has been performed using a inductively coupled plasma atomic emission spectrometer (ICP-AES). The spectral interferences of lithium content, 500, 1,000 and 2,000 mg/L, in the sample solution were investigated using an optimum wavelength for the respective metal species. As a result, the line intensities for Y, Nd, Sr, and La had no influences from the lithium content up to 2,000 mg/L, while Mo, Ba, Ru, Pd, Rh, Zr and Ce showed spectral interferences of 10% to 50%. The group separation of metals from lithium in the molten salts solution was carried out by adding ammonia water into the solution. The recovery of Ru, Y, Rh, Zr, Nd, Ce, La and Eu was found to be over 90%, while Mo, Ba, Pd, and Sr provided low recovery percentages.