• Journal of the Korean Crystal Growth and Crystal Technology
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• v.29 no.5
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• pp.222-228
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• 2019

In this study, we carried out the experiment to prepare lithium carbonate powder through gas-liquid reactions with a lithium-containing solution and $CO_2$ gas using lithium hydroxide, lithium chloride, and lithium sulfate. Thermodynamically, the carbonation reaction of a lithium-containing solution showed that aqueous reaction of lithium hydroxide occurs spontaneously, but aqueous reactions of lithium chloride and lithium sulfate does not occur spontaneously. In the case of lithium hydroxide solution, the recovery rate of lithium carbonate was 69.8 % at room temperature ($25^{\circ}C$), and increased to 89.4 % at $60^{\circ}C$. In the case of lithium chloride and lithium sulfate solution, lithium carbonate could be prepared using sodium hydroxide as an additive, but the recovery rates were 19.2 % and 16.7 %, respectively.

• 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.29 no.6
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• pp.27-34
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• 2020

In order to remove sulfate(SO42-) and purify the Li2CO3, dissolution and recrystallization of crude Li2CO3 using distilled water and HCl solution was performed. When Li2CO3 was dissolved using distilled water, the amount of dissolved Li2CO3(wt.%) increased as the solution temperature decrease and showed about 1.50 wt.% at 2.5℃. In addition, when Na2CO3 was added and the Li2CO3 solution was recrystallized, the recrystallization(%) increased with increasing temperature, resulting in a 49.00 % at 95 ℃. On the other hand, when Li2CO3 was dissolved using HCl solution, there was no effect of reaction temperature. As the concentration of HCl solution increased, the amount of dissolved Li2CO3(wt.%) increased, indicating 7.10 wt.% in 2.0 M HCl solution. When the LiCl solution was recrystallized by adding Na2CO3, it exhibited a recrystallization(%) of 86.10 % at a reaction temperature of 70 ℃, and showed a sulfate ion removal(%) of 96.50 % or more. Finally, more than 99.10 % of Na and more than 99.90 % of sulfate were removed from the recrystallized Li2CO3 powder through water washing, and purified Li2CO3 with a purity of 99.10 % could be recovered.

• Journal of Environmental Impact Assessment
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• v.32 no.2
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• pp.123-133
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• 2023

Wastewater generated in the secondary battery production process contains lithium and high-concentration sulfate. Recently, as demand as demand for high-Ni precursors with high-energy density has surged, nickel emission is also a concern. Lithium and sulfate are not included in the current water pollutant discharge standard, so if they are not properly processed and discharged, the negative effect on future environment may be great. Therefore, in this study, the ecotoxicity of lithium, nickel, and sulfate, which are potential contaminants that can be discharged from the secondary battery production process, was evaluated using water flea (Daphnia magna) and luminescent bacteria (Aliivibrio fischeri). As a result of the ecotoxicity test, 24-hour and 48-hour D. magna EC₅₀ values of lithium were 18.2mg/L and 14.5mg/L, nickel EC50 values were 7.2mg/L and 5.4mg/L, and sulfate EC₅₀ values were 4,605.5mg/L and 4,345.0mg/L, respectively. In the case of D. magna, it was found that there was a difference in ecotoxicity according to the contaminants and exposure time (24 hours, 48 hours). Comparing the EC₅₀ of D. magna for lithium, nickel, and sulfate, the EC₅₀ of nickel at 24h and 48h was 39.6-37.2% compared to lithium and 0.1-0.2% compared to sulfate, which was the most toxic among the three substances. The difference appeared to be at a similarlevelregardless of the exposure time. The EC₅₀ of sulfate was 253.0-299.7% and 639.5-804.6%, respectively, compared to lithium and nickel, showing the least toxicity among the three substances. The 30-minute EC₅₀ values of luminescent bacteria forlithium, nickel, and sulfate were 2,755.8mg/L, 7.4mg/L, and 66,047.3mg/L,respectively. Unlike nickel, it was confirmed that there was a difference in sensitivity between D. magna and A. fischeri bacteria to lithium and sulfate. Studies on the mixture toxicity of these substances are needed.

• The korean journal of orthodontics
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• v.28 no.6 s.71
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• pp.947-954
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• 1998

The purpose of this study was to compare shear bonding strengths and debonding patterns of the ceramic brackets attached on the crystal which were grown on the enamel surface of a tooth with different concentrations of lithium sulphate-contained polyacrylic acid in different application times. Four kinds of concentrations of mixed solutions were made and applied to the enamel surface on extracted human premolars. The solutions were made by adding 0.3M or 0.6M of lithium sulfate to $50\%\;or\;65\%$ of polyacrylic acid with 0.3M sulfuric acid. The solutions were applied for 30 or 60 seconds. After bonding, a universal testing machine was used to measure the shear bond strength, and then observations were made of debonding patterns through the stereoscope. And the enamel surface was observed through the scanning electron microscope to examine the pattern of crystal growth and debonding. The results were as follows: 1. Shear bond strength in the enamel surface treated with $50\%$ polyacrylic acid was higher than that with $65\%$ polyacrylic acid. 2. There were no statistical differences in shear bond strength according to concentration of lithium sulfate and application time of solutions . 3. Enamel surface was almost free of resin debris after debonding. 4. Enamel surface treated with $50\%$ polyacrylic acid showed higher density of crystal growth than that with $65\%$ polyacrylic acid under scanning electron microscope.

• 대한치과교정학회:학술대회논문집
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• 1998.10a
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• pp.77.3-77.3
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• 1998

• Resources Recycling
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• v.28 no.4
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• pp.51-58
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• 2019

Dismantlement of lithium primary batteries without explosion is required to recycle the lithium primary batteries which could be exploded by heating too much or crushing. In the present study, the optimum discharging condition was investigated to dismantle the batteries without explosion. When the batteries were discharged with $0.5kmol{\cdot}m^{-3}$ sulfuric acid, the reactivity of the batteries decreased after 4 days at $35^{\circ}C$ and after 1 day at $50^{\circ}C$, respectively. This result shows that higher temperature removed the high reactivity of the batteries. Because loss of metals recycled increases when the batteries are discharged only with the sulfuric acid, discharging process using acid solution and water was newly proposed. When the batteries were discharged with water during 24 hours after discharging with $0.5kmol{\cdot}m^{-3}$ sulfuric acid during 6 hours, the batteries discharged were dismantled without explosion. Because decrease in loss of metals was accomplished by new process, the recycling process of the batteries could become economic by the 2-step discharging process.

• 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.

• Resources Recycling
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• v.10 no.6
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• pp.9-14
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• 2001

A sulfuric acid leaching of $LiCoO_2$as cathodic active materials of lithium ion secondary batteries was investigated in terms of reaction variables. In the absence of a reducing agent, the extraction of cobalt was less than 40% in 2 M sulfuric acid at $75^{\circ}C$ instead of that of lithium could be almost 100% in the same conditions. To improve the Co extraction, hydrogen peroxide was used as a reducing agent in the range 2~20 vol%. When over 10vo1% hydrogen peroxide was added, the extractions of both metals were improved to about 95%. It seems to be due to the reduction of Co(III) to Co(II) that can be readily dissolved. The extractions of Co and Li were increased with increasing $H_2$$SO_4$concentration and temperature, and amount of hydrogen peroxide and with decreasing of pulp density. The optimum leaching conditions were determined at $2 M H_2$$SO_4$concentration, $75^{\circ}C$ operating temperature, 100 g/L. initial pulp density, 20 vol% $H_2$$O_2$addition and 30 min.

• Resources Recycling
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• v.31 no.4
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• pp.40-48
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• 2022

In waste lithium iron phosphate (LFP) batteries, the cathode material contains approximately 4% lithium. Recycling the constituent elements of batteries is important for resource circulation and for mitigating the environmental pollution. Li contained in the waste LFP cathode powder was selectively leached using persulfate-based oxidizing agents, such as sodium persulfate, potassium persulfate, and ammonium persulfate. Leaching efficiency and waste LFP powder properties were compared and analyzed. Pulp density was used as a variable during leaching, which was performed for 3 h under each condition. The leaching efficiency was calculated using the inductively coupled plasma (ICP) analysis of the leachate. All types of persulfate-based oxidizing agents used in this study showed a Li leaching efficiency over 92%. In particular, when leaching was performed using (NH₄)₂S₂O₈, the highest Li leaching percentage of 93.3% was observed, under the conditions of 50 g/L pulp density and an oxidizing agent concentration of 1.1 molar ratio.