• 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%).

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.32 no.2
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• pp.61-67
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• 2022

A metal salt solution was prepared from valuable metals (Ni, Co, Mn) recovered from a scrap of waste lithium secondary batteries, and an NCM811 precursor was synthesized from the solution. The effect on precursor formation according to reaction time was confirmed by SEM, PSA, and ICP analysis. Based on the analysis results, the electrochemical properties of the synthesized NCM811 precursor and the commercial NCM811 precursor were investigated. The Galvano charge-discharge cycle, rate performance, and Cycle performance were compared, and as a result, there was no significant difference from commercial precursors.

• Applied Chemistry for Engineering
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• v.34 no.5
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• pp.515-521
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• 2023

In this study, waste carbon fiber obtained by pyrolysis of carbon fiber reinforced plastic (CFRP) was used to produce carbon fluoride through vapor phase fluorination and recycled as a reducing electrode material for lithium primary batteries. First, the physicochemical properties of the waste carbon fiber obtained by pyrolysis were determined, and the structural and chemical properties of carbon fluoride were analyzed to evaluate the effect of vapor phase fluorination on the waste carbon fiber. XRD analysis confirmed that the hexagonal network carbon laminated structure (002 peak) of the waste carbon fiber was gradually converted into a carbon fluoride structure (CF_X, 001 peak) as the temperature of gas phase fluorination increased. The discharge capacity of the lithium primary battery produced using this carbon fluoride was up to 862 mAh/g. This was compared to the discharge capacity of carbon fluoride-based Li-ion batteries made of other carbon materials. These results suggest that carbon fluoride made from waste CFRP-based carbon fibers can be used as a reducing electrode material for Li-ion batteries.

• Resources Recycling
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• v.9 no.4
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• pp.37-43
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• 2000

Leaching of $LiCoO_2$ as a cathodic active materials for recovering Li and Co from spent lithium ion battery was investigated in terms of reaction variables. At the optimum condition determined in the previous work, Li and Co in a $H_2SO_4$ and $HNO_3$ solution were dissolved 70~80% and 40%, respectively. Li and Co were leached over 95% with the addition of a reductant such as $Na_2S_2O_3$ or $H_2O_2$. This behavior is probably due to the reduction of $Co^{3+}$ to $Co^{2+}$. Leaching of $LiCoCo_2$ powder obtained by calcination of an electrode materials from spent batteries was also carried out. Leaching efficiency of Li and Co were over 99% at the optimum condition with $H_2O_2$ addition of 1.7 vol.%. It seems to be due to the activation of $LiCoO_2$ by repeated charging and discharging or an imperfect crystal structure by deintercalation of Li.

• Clean Technology
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• v.26 no.2
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• pp.116-121
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• 2020

In this paper, the recycling of waste Ni-MH battery by-products for electric vehicle is studied. Although rare earths elements still exist in waste Ni-MH battery by-products, they are not valuable as materials in the form of by-products (such as an insoluble substance). This study investigates the recovering of rare earth oxide for solvent extraction A/O ratio, substitution reaction, and reaction temperature, and scrubbing of the rare earth elements for high purity separation. The by-product (in the form of rare earth elements insoluble powder) is converted into hydroxide form using 30% sodium hydroxide solution. The remaining impurities are purified using the difference in solubility of oxalic acid. Subsequently, Yttrium is isolated by means of D2EHPA (Di-[2-ethylhexyl] phosphoric acid). After cerium is separated using potassium permanganate, lanthanum and neodymium are separated using PC88A (2-ethylhexylphosphonic acid mono-2-ethylhexyl ester) and it is calcinated at a temperature of 800 ℃. As a result of the physical and chemical measurement of the calcined lanthanum and neodymium powder, it is confirmed that the powder is a microsized porous powder in an oxide form of 99.9% or more. Rare earth oxides are recovered from Ni-MH battery by-products through two solvent extraction processes and one oxidation process. This study has regenerated lanthanum and neodymium oxide as a useful material.

• Resources Recycling
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• v.15 no.6 s.74
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• pp.48-55
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• 2006

This study was carried out for establishing the physical recycling technique for commercializing process on household batteries. The procedure involves shape separator, crushing, magnetic separation, classification and eddy current separation in sequence. The separation capacity was 400-600 unit cell/hr with shape separation system. The impurities such as manganese and zinc in the magnetic product were below 0.1% respectively, the concentration of iron was above 99% in spent carbon zinc battery. Also non-magnetic products are composed of 22-30% En, 16-22% Mn, 1-3% Fe in the case oi spent zinc carbon battery. The amounts of other components such as carbon rod, plastics and separator were about 37-50%. From the eddy current separation of nonferrous products, the plate-type zinc components were separated up to 96% with 2,250-2,750 meter/min of the conveyor speed.

• 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.

• Journal of the Korean Society of Mineral and Energy Resources Engineers
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• v.55 no.6
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• pp.553-563
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• 2018

In this study, the location conditions and optimal technologies required for creating urban municipalities that can utilize the space in an abandoned mine area, where there is no infrastructure related to recycling wastes and valuable metals, are investigated. The urban mining industry deals with mineral resources through the processing of high value-added industrial by-products and wastes, and it is a useful linkage industry for the development of mineral resources and prevention of mining hazards. Urban mining technologies targeted at the abandoned mine area constitute screening, extraction, and smelting for recycling waste products. By analyzing the technologies available, an industrial network can be developed for recycling waste batteries and catalysts, which are promising raw materials. It is also important to establish an appropriate location for related industries that can generate value-added resources, rather than the resource supply and demand conditions seen in general urban mines. In order to overcome the accessibility and infrastructure limitations, the economic foundation of the abandoned mine area should consider the linkage of raw material supply, key technologies for recycling useful mineral resources that are derived from urban mines, spatial and site conditions, and industrial characteristics.

• New Physics: Sae Mulli
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• v.68 no.12
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• pp.1315-1323
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• 2018

We studied the carbonization due to the annealing condition of waste coffee powder for application as an active anode material for lithium-ion batteries (LIBs). The coffee powder used as an active anode material for LIBs was obtained from coffee beans, not from a coffee shells. The waste coffee powder was dried in air and heat-treated in an $Ar/H_2$ atmosphere to obtain a pore-forming activated carbon powder. The specific capacity of the sample annealed at $700^{\circ}C$ was still 303 mAh/g after 1000 cycles at a current density of 1000 mA/g and with a coulombic efficiency of over 99.5%. The number of pores and the pore size of the waste coffee powder were increased due to chemical treatment with KOH, which had the some effect as an increased specific surface area. The waste coffee powder is considered to be a very promising active anode material because of both its excellent electrochemical properties due to enhanced carrier conduction and its being a cost effective resource for use in LIBs.

• Resources Recycling
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• v.23 no.4
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• pp.21-29
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• 2014

Nickel, cobalt and manganese-based(NCM, $Li(Ni_xCo_yMn_z)O_2$) cathode active materials of spent lithium-ion batteries contained valuable metals such as cobalt(15 ~ 20%), nickel(25 ~ 30%), manganese(10 ~ 15%) and lithium(5 ~ 10%). It was investigated the eco-friendly leaching process for the recovery of valuable metal from spent lithium-ion battery NCM cathode active materials by DL-malic acid($C_4H_5O_6$) as an organic leachant in this research. The experiments were carried out to optimize the process parameters for the recovery of cobalt, nickel and lithium by varying the concentration of lixivant, reductant concentration, solid/liquid ratio and temperature. The leaching solution was analyzed using ICP-OES(Inductively Coupled Plasma Optic Emission Spectrometer). Cathode active materials of 5 wt. % were introduced into the leaching solution which was 2 M DL-malic acid in addition of 5 vol. % $H_2O_2$ at $80^{\circ}C$ and it resulted in the recovery of 99.10% cobalt, 99.80% nickel and 99.75% lithium in 120 min. $H_2O_2$ in DL-malic acid solution acts as an effective reducing agents, which enhance the leaching of metals.