• Membrane Journal
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• v.34 no.1
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• pp.1-9
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• 2024

The rapid expansion of the electric vehicle market has led to increased demand for battery recycling technologies. The recycling of spent batteries is crucial to stabilize the supply of rare metals, including lithium, cobalt and nickel, which are essential components for the battery industry. In addition, the technology for recycling spent batteries can help to reduce environmental and health impacts. This review presents the theoretical principles behind the metal recovery technology and the processes that are currently commercially available. It also describes trends in research and technological developments that aim to improve existing processes, and provides an overview of where recycling technology is headed.

• 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.

• Bulletin of the Korean Chemical Society
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• v.25 no.8
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• pp.1137-1142
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• 2004

A spectrophotometric and first derivative spectrophotometric method was developed in aquatic Tween 80 micellar solutions for selective determination of nickel without using any pre-separation step. 1-(2-Pyridylazo)-2-naphthol (PAN), as a sensitive chromogenic complexing agent formed a red-colored Ni(II)-PAN complex in Tween 80 media with satisfactory solubility and stability. Conditions such as pH, PAN concentration, type and concentration of micellizing agent were optimized. Molar absorptivity of Ni-PAN complex was found $4.62\;{\times}\;10^4L\;cm^{?1}\;mol^{?1}$ at 569 nm, under the optimum condition. Calibration graphs were derived by zero, first and second derivative spectrophotometry at maximum wavelengths of 569, 578 and 571 nm with linear ranges of 30-1800, 20-2500 and 30-2000 ng $mL^{?1}$ , respectively. Precision as standard deviation as well as accuracy as recovery percent were in the range of 1-20 ng $mL^{?1}$, and 93.3-103.3%, respectively, for the entire of the linear ranges. Spectrophotometric detection limit was 3 ng $mL^{?1}$ and effects of diverse ions on the first derivative determination of nickel were studied to investigate selectivity of the method. Interferences of cobalt and copper on the nickel determination were prevented using o-phenanthroline as masking agent. The recommended procedures were applied to the various synthetic and stainless steel alloys, tea leaves and human hair, with satisfactory results.

• Membrane and Water Treatment
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• v.10 no.2
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• pp.127-137
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• 2019

The D2EHPA/TBP co-extractants immobilized PolyHIPE membrane can be used for the selective separation of Mn (II) from Co (II). By solvent-nonsolvent method, D2EHPA/TBP co-extractants can be effectively immobilized into PolyHIPE membrane. The pore structure of PolyHIPE membrane and the presence of TBP enhance the stability of immobilized co-extractants. The optimal operating conditions for the separation of Mn (II) and Co (II) are feeding phase at pH 5.5, sulfuric acid concentration in the stripping phase of about 50 g/L and stirring speed at 400 rpm. The D2EHPA/TBP co-extractants ratio of 5:1 shows synergetic effect on Mn/Co separation factor about 22.74. The removal rate and recovery rate of Mn (II) is about 98.4 and 97.1%, respectively, while for Co (II) the transport efficiency is insignificant. The kinetic study of Mn (II) transport shows that high initial flux, $J_f^o=80.1({\mu}mol/m^2s)$, and maxima stripping flux, $J_s^{max}=20.8({\mu}mol/m^2s)$, can be achieved with D2EHPA/TBP co-extractants immobilized PolyHIPE membrane. The stability and reusability study shows that the membrane can maintain a long term performance with high efficiency. High purity of Co (II) and Mn (II) can be recovered from the feeding phase and stripping phase, respectively.

• Analytical Science and Technology
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• v.20 no.6
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• pp.496-501
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• 2007

The 242.795 nm on ICP-AES for the gold analysis was the most sensitive wavelength which was also interfered severely by the spectra of other metal ions such as manganese, chromium, cobalt, and iron. In order to analyze the gold in ore, the gold must be separated from the interfering ions. The best solvent for separation of gold in ore solution was 10 % n-hexane contained MIBK mixed solvent. The gold recovery was 97.5 % from mixed metal solution contained about 2 M $HNO_3$ and 0.5 M HCl.

• Resources Recycling
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• v.23 no.1
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• pp.64-69
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• 2014

For the recovery of Co and Cu, bioleaching behavior of Co, Cu, Fe, Mg, Al by Aspergillus niger culture from the molasses growth medium was investigated. Series of leaching tests have been conducted by varying Aspergillus niger's type, molasses concentration in the growth medium, pulp density and reaction time. The results showed that increase of the molasses concentration in the growth medium from 1% to 4% increased the leaching percentage of Co and Cu and the optimal molesses concentration was found to be 4% in the growth medium. Maxinum 90% of Co and 70% of Cu were dissolved from the leaching test at the 10 g/L pulp density, 4 % of molasses concentration in the growth medium after 21 days by Aspergillus niger KCTC 6985. But in case of using Aspergillus niger KCTC 6144, the maxium leaching percentage of Co and Cu was reached 90% respectively at a pulp density 5 g/L and 4% of molasses concentration.

• Bulletin of the Korean Chemical Society
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• v.27 no.9
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• pp.1293-1296
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• 2006

In this study, a solid phase extraction method has been developed for the preconcentration and separation of the elements Cr(III), Fe(III), Co(II) and Pb(II) at trace levels by using a column packed with Amberlite XAD-1180 resin loaded with 4-(2-pyridylazo)-resorcinol (PAR) reagent. After preconcentrating, the metals retained on the column were eluted with 20 mL of 3 mol/L $HNO_3$ and then determined by flame atomic absorption spectrometry (FAAS). The factors affecting the recovery of the elements, such as pH, type and concentration of eluent, volume of sample and elution solution, and matrix components, were also ascertained. The recoveries of Cr(III), Fe(III), Co(II) and Pb(II) were found to be $99\;{\pm}\;4,\;97\;{\pm}\;3,\;95\;{\pm}\;3$ and $98\;{\pm}\;4$%, respectively, under the optimum conditions at 95% confidence level and the relative standard deviations found by analyzing of nine replicates were $\leq4.4$%. The preconcentration factors for Cr(III), Fe(III), Co(II) and Pb(II) were found as 75, 125, 50 and 75 respectively. The detection limits (DL, 3s/b) were 3.0 $\mu g/L$ for Cr(III), 1.25 $\mu g/L$ for Fe(III), 3.3 $\mu g/L$ for Co(II), and 7.2 $\mu g/L$ for Pb(II). The recoveries achieved by adding of metals at known concentrations to samples and the analysis results of Buffalo river sediment (RM 8704) show that the described method has a good accuracy. The proposed method was applied to tap water, stream water, salt and street dust samples.

• Bulletin of the Korean Chemical Society
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• v.27 no.11
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• pp.1757-1762
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• 2006

A solvent sublation using salphen as a ligand was studied and applied for the determination of trace Ni(II), Co(II) and Cu(II) in water samples. The fundamental study was investigated by a solvent extraction process because the solvent sublation was done by extracting the floated analytes into an organic solvent from the aqueous solution. The salphen complexes of Ni(II), Co(II) and Cu(II) ions were formed in an alkaline solution of more than pH 8 and then they were extracted into m-xylene. It was known that the each metallic ion formed 1 : 1 complex with the salphen and the logarithmic values of extraction constants for the complexes were 3.3 5.1 as an average value. Based on the preliminary study, the procedure was fixed for the separation and concentration of the analytes in samples. Various conditions such as the pH of solutions, the influence of $NaClO_4$, the bubbling rate and time of $N_2$ gas, and the type of organic solvent were optimized. The metal-salphen complexes could be extracted into m-xylene from the solution of more than pH 8, but the pH could be shifted to acidic solution of pH 6 by the addition of $NaClO_4$. In addition, the solvent sublation efficiency of the analytes was increased by adding $NaClO_4$. The recovery of 97-115% was obtained in the spiked samples in which given amounts of 0.3 mg/L Ni(II), 0.8 mg/L Co(II) and 0.04 mg/L Cu(II) were added.

• 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.

• Resources Recycling
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• v.30 no.6
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• pp.28-35
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• 2021

An experiment was conducted to separate or recover Co and Ni using Cyanex 301 from process by-products and waste resources containing Co and Ni. To separate and recover Co and Ni from simulated leaching solutions, 10 v/v% Cyanex 301 was used as an extractant in this study; Li was not extracted. At equilibrium pH 1.5 and a phase ratio (A/O) of 1.0, 0.44% of Mg and 11.57% of Mn were extracted, and more than 99% of Co and Ni were extracted. McCabe-Thiele diagram analysis confirmed that more than 99.9% of Co and Ni could be extracted simultaneously through two-stage extraction with an extraction phase ratio (A/O) of 2. It was possible to extract Mg and Mn simultaneously through the scrubbing process. In the scrubbing process, more than 99% of Mg and 87% of Mn were scrubbed using 0.05 M of H₂SO₄, and 99.9% of Mg and more than 80% of Mn were scrubbed using 0.05 M of HCl. In the stripping process, 93% of Co and 5% of Ni were stripped selectively by 3.0 M of H₂SO₄. However, when 8.0 M of HCl was used as a stripping solution, more than 99.9% of Co and more than 90% of Ni were stripped simultaneously.