• 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.30 no.5
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• pp.57-66
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• 2021

In this study, we attempted to separate and recover Cu from low-grade copper ore by a hydrometallurgical process. The leaching sample obtained after crushing and sieving by 0.355 mm of low-grade copper ore contained 1.5% Cu, 4.7% Fe, 1.0% Mn, and 0.3% Zn. The Cu in the oxide ore was very well leached into sulfuric acid and 97% Cu leaching efficiency was achieved at 80℃ and 3 M sulfuric acid (H₂SO₄). From the leaching solution, Cu was separated by solvent extraction from Fe, Mn, and Zn using LIX984N. The separation tendency between Cu and other metals was confirmed through the distribution ratio and separation factor. By plotting the McCabe-Thiele Diagram, the optimum condition for recovering Cu is 5 vol.% LIX984N, 2-stage counter-current solvent extraction, and an O/A ratio of 0.5. Using this method, 99% of the Cu was extracted and a CuSO₄ solution was finally obtained that contained 1.6 g/L Cu after the stripping process using 2 M H₂SO₄.

• Resources Recycling
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• v.30 no.4
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• pp.11-19
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• 2021

Arsenic (As) oxidation followed by precipitation from a high-As(III)-containing leaching solution derived from a sulfidic ore was investigated in this study to remove aqueous As from the solution using activated carbon (AC) with air injection as an oxidant. To obtain the initial leaching solution, a domestic sulfidic ore was leached in a sulfuric acid solution at pH 1 and 50℃ for 95 h, and approximately 7 g/L of Fe and 3 g/L of As were leached out. To determine the effect of the oxidative reaction utilizing AC with air injection, the leaching solution was tested under the following five oxidative conditions at an initial pH of 1 and 90℃ for 72 h: air-only injection; air injection with 1, 5, and 10 w/v% of AC addition; and H₂O₂ addition. The tests in the presence of both air and AC revealed that the oxidation kinetics and As removal were improved by the reaction between the metallic species and the surface group formed on the AC surface. In addition, the greater the amount of AC added, the better was the reaction efficiency, removing 93-94% of As with more than 5 w/v% of AC addition. Finally, X-ray diffraction analysis confirmed that the precipitate formed from the oxidative reaction was scorodite (FeAsO₄·2H₂O).

• Resources Recycling
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• v.31 no.4
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• pp.49-55
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• 2022

In this study, the heavy metal ions (of Pb, Cd, Cr, and Hg) in wastewater were removed using a spent Li₂O-Al₂O₃-SiO₂-based crystallized glass previously used as an induction top plate material. Changes in the removal efficiency of heavy metals according to different reaction parameters, such as the amount of zeolite used as a heavy-metal adsorbent, adsorption time, initial concentration of the heavy metals, and pH of the initial solution, were investigated. As the amount of zeolite added increased, the heavy-metal removal efficiency also increased. Adsorption time had a considerable influence on adsorption characteristics, and the removal efficiency of all heavy metals increased with increasing adsorption time. In the case of Cd, the removal efficiency was greatly improved depending on the adsorption time. The initial concentration of the heavy-metal solution did not affect the removal efficiency; however, the initial pH of the heavy-metal solution affected the removal efficiency. More specifically, the removal efficiency of Cd increased while that of Pb and Cr decreased with increasing pH. The adsorption characteristics of Hg were not significantly affected by pH.

• Resources Recycling
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• v.31 no.4
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• pp.19-25
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• 2022

In this study, tungsten carbide (WC) powder was prepared using a novel recycling process for hard metal sludge that does not use ammonium paratungstate. Instead of ammonia, acid was used to remove the sodium and crystallized tungstate, resulting in the formation of tungstic acid (H₂WO₄). The WC powder was successfully synthesized by the carbothermal reduction of tungstic acid through H₂O decomposition, reduction of WO₃ to W, and formation of WC. The carbon content and holding time at the carbothermal reduction temperature were optimized to remove free carbon from the WC powder. As a result, most of the free carbon in the WC powder prepared from sludge was removed, and the content of free carbon in the synthesized WC powder was lower than that in commercial WC powder. Moreover, the crystallite size of WC prepared from H₂WO₄ was much smaller than that of commercial micron-sized WC powder produced from APT. The small crystallite size of WC induces grain growth during the sintering of the WC-Co composite; thus, a WC-Co composite with large WC grains was fabricated using the WC powder prepared from H₂WO₄. The large WC grains affected the mechanical properties of the WC-Co composite. Further, due to the large grain size, the WC-Co composite fabricated from H₂WO₄ exhibited a higher toughness than that of the WC-Co composite prepared from commercial WC powder.

• Resources Recycling
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• v.30 no.2
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• pp.39-45
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• 2021

Spent photovoltaic module is one of the important resource of silver, while related research concerning silver recovery remains limited. In our previous research, HNO3 was utilized to dissolve Ag(I) and Al(III) from the spent silicon solar cells. In order to recover Ag(I) from the leachate of a silicon solar cell, the present study made use of a nitrate solution containing Ag(I) and Al(III), which was subjected to a solvent extraction process with 5,8-diethyl-7-hydroxydodecan-6-oxime (LIX63). Ag(I) was selectively extracted with LIX63 over Al(III) from the nitrate leach solution. Subsequently, quantitative stripping of Ag(I) from the loaded LIX63 was performed by using 20% ammonia water. The McCabe-Thiele plots for the extraction and stripping isotherms of Ag(I) were also constructed. Extraction and stripping simulation tests confirmed an Ag(I) extraction and stripping efficiency of >99.99% and 98.9%, respectively with high purity Ag (99.998%) and Al (99.99%) solution. A process flow sheet for Ag(I) recovery from the nitrate leach solution was proposed.

• Resources Recycling
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• v.31 no.5
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• pp.34-41
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• 2022

Smelting reduction of spent lithium-ion batteries results in metallic alloys, slag, and dust containing Li(I). Precipitation of Li₂CO₃ was performed using the synthetic leachate of the dust. Herein, the effects of the precipitant and addition of non-aqueous solvents on the precipitation of Li(I) were investigated. Na₂CO₃ was a more effective precipitating agent than (NH₄)₂CO₃ owing to the hydrolysis reaction of dissolved ammonium and carbonate. The addition of acetone or ethanol improved the Li(I) precipitation percentage for both the precipitants. When using (NH₄)₂CO₃, the Li(I) precipitation percentage increased at a solution pH of 12. Under the same conditions, the Li(I) precipitation percentage using Na₂CO₃ was much higher than that using (NH₄)₂CO₃.

• Resources Recycling
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• v.31 no.3
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• pp.81-87
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• 2022

Energy consumption per unit weight of metal (kwh/kg of metal) is one of the most important economic indicators in the process of molten salt electrolysis. It is related to the heat loss of salt bath and the current efficiency of the process. The current efficiency is highly dependent on electrolysis temperature. On the other hand, the temperature of salt bath may increase significantly due to the difference (larger energy input than consumption) in heat balance at the beginning of electrolysis, which may cause different electrolysis temperature from an initially targeted value. This results in a bad effect on current efficiency. Therefore, it will be helpful to the reduction of energy consumption to compare the calculated and measured values of the temperature change of salt bath through the heat balance review at the early stage of electrolysis and to evaluate the energy loss to outside. In this study, based on the authors' experimental data, the heat balance was reviewed at the beginning of the electrolysis, and it was possible to evaluate the energy loss to the outside and the increase of the temperature of the salt bath quantitatively. Through such a method, heat loss reduction plan can be derived and current efficiency can be improved so that energy consumption can be reduced.

• Resources Recycling
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• v.31 no.6
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• pp.81-91
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• 2022

The use of lithium-ion batteries increases significantly with the rapid spread of electronic devices and electric vehicle and thereby an increase in the amount of waste batteries is expected in the near future. Therefore, studies are continuously being conducted to recover various resources of cathode active material (Ni, Co, Mn, Li) from waste battery. In order to recover the cathode active material, black mass is generally recovered from waste battery. The general process of recovering black mass is a waste battery collection - discharge - dismantling - crushing - classification process. This study focus on the crushing/classification process among the processes. Specifically, the particle size distribution of various samples at each crushing/classification step were evaluated, and the particle shape of each particle fraction was analyzed with a microscope and SEM (Scanning Electron Microscopy)-EDS(Energy Dispersive Spectrometer). As a result, among the black mass particle, fine particle less than 74 ㎛ was the mixture of cathode and anode active material which are properly liberated from the current metals. However, coarse particle larger than 100 ㎛ was present in a form in which the current metal and active material were combined. In addition, this study developed a PBM(Population Balance Model) system that can simulate two-species mixture sample with two different crushing properties. Using developed model, the breakage parameters of two species was derived and predictive performance of breakage distribution was verified.

• Resources Recycling
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• v.32 no.6
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• pp.25-33
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• 2023

With the growth of the battery industry, a rapid increase in the production and usage of lithium-ion batteries is expected, and in line with this, much interest and effort is being paid to recycle waste batteries, including production scrap. Although much effort has been made to recycle cathode material, much attention has begun to recycle anode material to secure the supply chain of critical minerals and improve recycling rates. The proximate analysis that measures the content of coal can be used to analyze graphite in anode material, but it cannot accurately analyze due to the interaction between the components of the black mass. Therefore, in this study, thermogravimetric analysis of each component of black mass was measured as the temperature increased up to 950℃ in an oxygen atmosphere. As a result, in the case of cathode material, no change in mass was measured other than a mass reduction of about 5% due to oxidation of the binder and conductive material. In the case of anode material, except for a mass reduction of about 2% due to the binder, all mass reduction were due to the graphite(fixed carbon). In addition, metal conductors (Al, Cu) were oxidized and their mass increased as the temperature increased. Thermal analysis results of mixed samples of cathode/anode show similar results to the predictive values that can be calculated through each cathode and anode analysis results.