• Resources Recycling
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• v.33 no.3
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• pp.21-29
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• 2024

Globally, the demand for electric vehicles (EVs) is surging due to carbon-neutral strategies aimed at decarbonization. Consequently, the demand for lithium-ion batteries, which are essential components of EVs, is also rising, leading to an increase in the generation of spent batteries. This has prompted research into the recycling of spent batteries to recover valuable metals. In this study, we aimed to selectively leach and recover lithium from the cathode material of spent LFP batteries. To enhance the reaction surface area and reactivity, the binder in the cathode material powder was removed, and the material was subjected to heat treatment in both atmospheric and nitrogen environments across various temperature ranges. This was followed by a mechanochemical process for aqueous leaching. Initially, after heat treatment, the powder was converted into a soluble lithium compound using sodium persulfate (Na₂S₂O₈) in a mechanochemical reaction. Subsequently, aqueous leaching was performed using distilled water. This study confirmed the changes in the characteristics of the cathode material powder due to heat treatment. The final heat treatment in a nitrogen atmosphere resulted in a lithium leaching efficiency of approximately 100% across all temperature ranges.

• Resources Recycling
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• v.14 no.6 s.68
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• pp.28-36
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• 2005

A hydrometallurgical process to leach cobalt from the waste cathodic active material, $LiCoO_{2}$, and subsequently to separate it by solvent extraction was developed. The optimum leaching conditions for high recovery of colbalt and lithium were obtained: 2.0 M sulfuric acid, 5 $vol.\%$ hydrogen peroxide, $75^{\circ}C$ leaching temperature, 30 minutes leaching time and an initial pulp density of 100 g/L. The respective leaching efficiencies for Co and Li were $93\%$ and $94.5\%$. About $85\%$ Co was extracted from the sulfuric acid leach liquor containing 44.72 g/L Co and 5.43 g/L Li, using 1.5 M Cyanex272 as an extractant at the initial pH 5.0 and in organic to aqueous phase ratio of 1.6:1 under the single stage extraction conditions. The Co in the raraffinate was completely extracted by 0.5 M Na-Cyanex272 at the inital pH 5.0, and an organic to aqueous phase ratio of 1;1. The cobalt sulfate solution of higher than $99.99\%$ purity could be recovered from waste $LiCoO_{2}$, using a series of hydrometallurgical processes: sulfuric acid leaching of waste $LiCoO_{2}$- solvent extraction of Co by Na-Cyanex 271 - scrubbing of Li by sodium carbonate solution - stripping of Co by sulfuric acid solution.

• Polymer(Korea)
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• v.31 no.4
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• pp.297-301
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• 2007

In this work, polymer/(layered silicate) nanocomposites (PLSN) based on poly (ethylene oxide) (PEO), ethylene carbonate (EC) as a plasticizer, lithium salt ($LiClO_4$), and sodium montmorillonite ($Na^+-MMT$) or organic montmorillonite (organic MMT) clay were fabricated. And the effects of organic MMT on the polymer matrix were investigated as a function of ionic conductivity. For the application to electrolytes an Li batteries, polymer electrolytes containing the organic nanoclays were used in this work. As a result, the spacing between layers and hydrophobicity of the organic nanoclays were increased, affecting on the exfoliation behaviors of the MMT layers in clay/PEO nanocomposites. From ion-conductivity results, the organic-MMT showed higher values than those of $Na^+-MMT$, and the MMT-20A sample that was treated by methyl dihydrogenated tallow ammonium, showed the highest conductivity in this system.

• 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%).

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.11a
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• pp.259-259
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• 2007

층상구조의 전이금속 산화물($LiMO_2$, M=Co, Ni, Mn)은 리튬이차전지용 양극재료로 활발한 연구가 진행되고 있다. 차세대 리튬이차전지 시스템의 개발 및 고성능화를 위해서는 전지의 용량을 결정하는 핵심 부품인 양극재료의 고용량화 및 고안정화는 필수 불가결하다. 따라서 본 연구에서는 상업적으로 큰 장점이 있는 고상반응 공정을 이용하여 리튬이차전지용 양극소재를 제조하고, 소재의 전기화학적, 구조적인 특성을 평가하였으며, 다음과 같은 주제를 가지고 연구를 진행하였다. $LiCoO_2$ 양극재료는 리튬이온전지로 널리 사용되고 있다. 높은 에너지 밀도의 리튬이온전지를 얻기 위해서는 $LiCoO_2$ 양극재료가 고용량화 및 고밀도화를 가져야 한다. 여기서 $LiCoO_2$ 분말이 irregular particle morphology를 가지면 tap density가 $2.2-2.4gcm^{-3}$로 에너지 밀도가 낮으나, 구형 $LiCoO_2$의 정극재료는 tap density가 $2.6-2.8gcm^{-3}$로 상대적으로 energy density가 높아지는 효과가 있다. 구형 $LiCoO_2$ 양극재료를 합성하기 위해서는 chelating agent를 이용한 "controlled crystallization" 침전법을 사용하여 합성한 구형 코발트 수화물을 사용하고 있다. "controlled crystallization" 침전법에서 사용되는 chelating agent로는 주로 ammonia가 이용되고 있다. 본 연구에서는 chelating agent로 ethylene diamine을 사용하여 sodium hydroxides를 precipitation으로 침전 반응하여 구형 코발트 수화물을 합성하였다. 상기 방법으로 합성된 코발트 수화물과 리튬 수화물($LiOH{\cdot}H_2O$-고순도화학(高殉道化學))을 사용하여 고상법을 통하여 $LiCoO_2$를 합성하였다. 제조된 분말의 결정구조와 전기화학적 특성분석은 X-선 회절분석 및 리트벨트 구조정산, 그리고 충/방전 싸이클링을 수행하였으며, 분말의 미세구조 변화를 SEM을 이용하여 분석하였다.