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Recovery of iron phosphate and lithium carbonate from sulfuric acid leaching solutions of spent LiFePO4 batteries by chemical precipitation

Jing Chen, Tran Thanh Tuan, Lee Man Seung

Physicochemical Problems of Mineral Processing

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2024

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Vol. 60, iss. 3

art. no. 189463

EN

The recycling of lithium and iron from spent lithium iron phosphate (LiFePO4) batteries has gained attention due to the explosive growth of the electric vehicle market. To recover both of these metal ions from the sulfuric acid leaching solution of spent LiFePO4 batteries, a process based on precipitation was proposed in this study. Since ferric and ferrous ions coexisted in the leaching solution, all the ferrous ions were first oxidized to ferric ions by adding H2O2 to the leaching solution. About 99% iron(III) was recovered as iron phosphate by adjusting the solution pH to 2 at 25°C for 30 mins. After the precipitation of iron phosphate, the remaining Li(I) in the filtrate was recovered as lithium carbonate by precipitation with Na2CO3 as a precipitant. Addition of acetone to the filtrate at room temperature greatly enhanced the precipitation percentage of Li(I). Moreover, solid Na2CO3 was better than Na2CO3 solution in precipitating Li(I). About 95% of lithium ions was recovered as carbonate precipitates under the optimum conditions: solution pH = 11, 3.0 molar ratio of solid Na2CO3 to Li(I), 7/5(v/v) volume ratio of acetone to the filtrate, 25°C, 300 rpm for 2 hrs.

2

Comparison of separation of Mn(II), Co(II), and Ni(II) by oxidative precipitation between chloride and sulfate solutions

Wen Jiangxian, Tran Thanh Tuan, Lee Man Seung

Physicochemical Problems of Mineral Processing

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2024

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Vol. 60, iss. 1

art. no. 183029

EN

In hydrometallurgy, precipitation would be easier and simpler than solvent extraction as a separation operation. In this work, the separation performance of Co(II), Mn(II) and Ni(II) by oxidative precipitation was investigated. For this purpose, NaClO was employed as an oxidizing agent and the separation behavior of the three ions was compared between chloride and sulfate solutions by varying some factors such as the dosage of NaClO, solution pH and reaction temperature. By controlling the molar ratio of NaClO to Mn(II), Mn(II) were easily separated as MnO2 by oxidative precipitation from both chloride and sulfate solutions. At the same experimental conditions, precipitation percentage of Co(II) from chloride solution was higher than that from sulfate solution, which can be ascribed to the stronger tendency of Co(II) to form complexes with chloride ion than with sulfate ions. Addition of NaCl to sulfate solution and oxidative precipitation at high temperature enhanced the precipitation percentage of Co2O3 and thus separation degree between Co(II) and Ni(II) was improved. Under the optimum conditions, MnO2 and Co2O3 powders with 99.9% purity were completely recovered by oxidative precipitation from chloride solution. By contrast, the purities of the MnO2 and Co2O3 thus recovered from sulfate solution were only 76 and 91%, respectively. Our results indicated that chloride solution would be more effective than sulfate solution in separating Mn(II) and Co(II) by oxidative precipitation with NaClO. Therefore, the use of chloride-based leaching solutions such as HCl and FeCl3 might be better for the leaching medium of spent lithium-ion batteries.

3

A hydrometallurgical process for the recovery of copper metal and nickel hydroxide from the aqua regia leaching solutions of printed circuit boards

Nguyen Thi Nhan Hau, Wen Jiangxian, Lee Man Seung

Physicochemical Problems of Mineral Processing

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2024

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Vol. 60, iss. 4

art. no. 191551

EN

Leaching solutions of printed circuit boards (PCBs) contain noble and base metal ions. The precious metal ions present in the leaching solutions of PCBs could be separated by cementation with copper metal. After recovery of precious metal ions by cementation, the filtrate contains Cu(II) together with base metal ions like Al(III), Fe(III), Fe(II), Ni(II), Sn(II), and Zn(II). In this work, separation experiments were conducted to recover Cu(II) and Ni(II) from the filtrate. First, copper ions were completely separated from the filtrate by chemical reduction with hydrazine at the following conditions: a molar ratio of 8 for hydrazine to Cu(II), 20°C, 500 rpm, and 20 mins. By adding sodium oxalate to the solution after separation of Cu(II), most of the Ni(II) and 38% of the Zn(II) were co-precipitated at 20°C, 60 mins, 500 rpm, and a molar ratio of 20 for sodium oxalate to nickel. After dissolving the coprecipitates of Ni(II) and Zn(II) oxalates in a 0.5 M HCl solution, the Zn(II) was completely removed from the solution by a five-stage cross-current extraction with 2.5 M Cyanex 272. Nickel hydroxides were then recovered from the raffinate by precipitation with NaOH. The purity of the copper metal and nickel hydroxides was higher than 99%. A process was proposed to recover Au(III), Pd(II), Cu(II), and Ni(II) from the leaching solutions of PCBs.

4

Solvent extraction of Terbium(III) from chloride solution using organophosphorus extractant, its mixture and ionic liquid in the presence of organic acids

Tran Thanh Tuan, Song Si Jeong, Oh Chang Geun, Lee Man Seung

Physicochemical Problems of Mineral Processing

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2023

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Vol. 59, iss. 2

art. no. 162714

EN

Addition of organic acids to dilute hydrochloric acid solution can improve the extraction of rare earth elements by single cationic extractants. However, the correlation between the chemical structure of organic acids and the extraction of REEs as well as the variation in equilibrium pH has not been elucidated. In this study, we investigated the extraction of Tb(III) from dilute HCl solutions containing an organic acid like formic, lactic, fumaric, or maleic acid. As extractants, single Cyanex 272, a mixture of Cyanex 272 and Alamine 336 (Ala336-Cy272), and an ionic liquid (ALi-Cy272) synthesized by Cyanex 272 and Aliquat 336 were used. The speciation of Tb(III) in dilute HCl solutions containing organic acids was analyzed. In extraction of Tb(III), organic acids showed two roles as complexing and buffering agent, which depended on the chemical structure of the acids. There was some difference in the extraction of Tb(III) between single Cyanex 272 and ionic liquid, ALi-Cy272. During extraction with ALi-Cy272, formic and lactic acid negatively affected the extraction of Tb(III). The fact that the chemical structure of organic acids affected the extraction of Tb(III) from dilute HCl solution by the studied extractants can provide important information on the selection of suitable extraction systems.

5

Recovery of pure palladium compound from the spent electroplating solutions by hydrometallurgical method

Nguyen Viet Nhan Hoa, Song Si Jeong, Lee Man Seung

Physicochemical Problems of Mineral Processing

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2022

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Vol. 58, iss. 1

88--100

EN

Electroplating of palladium (Pd) is practiced in the manufacture of electronic materials. The increasing demand for Pd metal necessitates the recovery of Pd(II) from the spent electroplating solutions. In this work, the recovery of Pd compound was studied from the cemented Pd by zinc (Zn) metal from spent electroplating solutions. Initially, the selective extraction ability of ionic liquids synthesized from commercial extractants for Pd(II) over Zn(II) from the synthetic HCl solution was investigated. Pd(II) was selectively extracted over Zn(II) from 9 M HCl solution by ALi-CY301(Nmethyl-N,N,N-trioctylammonium bis(2,4,4-trimethylpentyl) dithiophosphinic) and by ALi-I (N-methylN,N,N-trioctylammonium iodide) from weak HCl solution (pH 1). Since 9 M HCl was needed to completely dissolve Pd from the cemented Pd, ALi-CY301 was employed for the separation of Pd(II) and Zn(II) from the real HCl leaching solution of the cemented Pd. Two-stages counter-current extraction of the real HCl solution with ALi-CY301 resulted in selective extraction of Pd(II). Pd(II) was effectively stripped from the loaded ALi-CY301 by a mixture of HCl and NaClO. After oxidizing Pd(II) in the stripping solution to Pd(IV) by adding NaClO, Pd(IV) compound was synthesized by adding NH4Cl as a precipitant. By comparing leaching and extraction efficiency between hydrochloric and sulfuric acid solutions, a hydrometallurgical process consisted of HCl leaching, extraction with ALiCY301 and precipitation with NH4Cl was recommended for the recovery of pure (NH4)2PdCl6 from the cemented Pd.

6

Improvement of metal separation process from synthetic hydrochloric acid leaching solution of spent lithium ion batteries by solvent extraction and ion exchange

Nguyen Viet Nhan Hoa, Lee Man Seung

Physicochemical Problems of Mineral Processing

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2021

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Vol. 57, iss. 4

1--17

EN

Spent lithium-ion batteries (LIBs) are good secondary resources for recycle and reuse. To develop a process for the separation of Cu(II), Co(II), Mn(II), Ni(II) and Li(I) with high purity from spent LIBs and circumvent some drawbacks of the previous work, solvent extraction and ion exchange experiments were done in this work. The synthetic hydrochloric acid leaching solution of 3 M was employed. Compared to Aliquat 336 (N-Methyl- N, N, N-trioctyl ammonium chloride), extraction with Cyanex 301 (bis(2,4,4-trimethylpentyl) dithiophosphinic acid) led to selective extraction of Cu(II) over other metal ions. Employing ion exchange with TEVA-SCN resin can completely separate Co(II) over Mn(II). After adjusting the pH of Co(II) free raffinate to 3, Mn(II) was quantitatively extracted by the mixture of Alamine 336 (mixture of tri-octyl/decyl amine) and PC 88A (2-ethylhexyl hydrogen-2-ethylhexylphosphonate) with two stage cross-current extraction. The synthesized ionic liquid (ALi-CY) was used for complete extraction of Ni(II), whereas Li(I) remained in final raffinate. The metal ions in the loaded organic phase were completely stripped with the proper agents (5% aqua regia for Cu(II), 5% NH3 for Co(II), weak H2SO4 solution for Mn(II) and Ni(II) stripping, respectively). The experimental results revealed that purity of the metal ions in stripping solution was higher than 99.9%. A flowsheet was suggested to separate metal ions from the HCl leaching solutions of spent LIBs.

7

Study on Recovery of Valuable Metals in Spent Lithium-Ion Batteries by Al2O3-SiO2-CaO-Fe2O3 Slag System

Moon Tae Boong, Han Chulwoong, Hyun Soong-Keun, Park Sung Cheol, Son Seong Ho, Lee Man Seung, Kim Yong Hwan

Archives of Metallurgy and Materials

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2021

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Vol. 66, iss. 4

983--986

EN

This study investigated the recovery behavior of valuable metals (Co, Ni, Cu and Mn) in spent lithium ion-batteries based on Al2O3-SiO2-CaO-Fe2O3 slag system via DC submerged arc smelting process. The valuable metals were recovered by 93.9% at the 1250°C for 30 min on the 20 Al2O3-40SiO2-20Cao-20Fe2O3 (mass%) slag system. From the analysis of the slag by Fourier-transform infrared spectroscopy, it was considered that Fe2O2 and Al2O3 acted as basic oxides to depolymerize SiO4 and AlO4 under the addition of critical 20 mass% Fe2O3 in 20 Al2O3-40SiO2-Cao-Fe2O3 (Cao + Fe2O3 = 40 mass%). in addition, it was observed that the addition of Fe2O3 ranging between 20 and 30 mass% lowers the melting point of the slag system.

8

Effect of Flux on the Recovery Behavior of Valuable Metals during the Melting Process of Aluminum Can Scrap

Han Chulwoong, Kim Yong Hwan, Kim Dae-Geun, Lee Man Seung

Archives of Metallurgy and Materials

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2021

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Vol. 66, iss. 4

1023--1027

EN

This study investigated the effect of flux type and amounts on recovery behavior of aluminum alloy during the melting process of Al can scrap. The heat treatment was conducted to remove the coating layer on the surface of can scrap at 500°C for 30 min. The molten metal treatment of the scrap was performed at 750°C in a high-frequency induction furnace with different flux types and amounts. It was observed that the optimum condition for recovery of Al alloy was to add about 3 wt.% flux with a salt and MgCl2 mixing ratio of 70:30 during melting process. The mechanical properties of recovered Al alloy were about 254.8 mPa, which is similar to that of the virgin Al5083 alloy.

9

Separation of rare earth elements from the leaching solution of waste phosphors by solvent extraction with Cyanex 272 and its mixture with Alamine 336

Xing Weidong, Lee Man Seung

Physicochemical Problems of Mineral Processing

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2020

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Vol. 56, iss. 1

184--194

EN

Waste phosphors contain rare earth elements (REEs) such as yttrium (Y), europium (Eu), cerium (Ce), terbium (Tb) and lanthanum (La). Separation of these REEs from the leaching solution of waste phosphors was investigated by solvent extraction with single Cyanex 272, binary mixture (mixture of Cyanex 272 and Alamine 336), ionic liquid (prepared by Cyanex 272 and Aliquat 336) in kerosene. The effect of solution pH and extractants concentration was mainly investigated. The results indicated that Y(III) was selectively extracted by single Cyanex 272 over the other four REEs from the HCl solution with initial pH range from 3 to 5. Synergistic extraction with the binary mixture was enough for the extraction of Y(III), Tb(III) and Eu(III) with a small amount of Ce(III). Scrubbing with pure Y(III) solution with intermediate acidity was effective in scrubbing Ce(III) from the loaded binary mixture organic phase. Stripping behavior of the Y(III), Tb(III) and Eu(III) by HCl solution was similar to each other. Tb(III) and Eu(III) can be separated by extraction with the binary mixture followed by scrubbing with pure Tb(III) solution. McCabe-Thiele diagrams were constructed for the extraction of Y(III) by single Cyanex 272 and that of Tb(III) by the mixture. A process was proposed for the separation of REEs from the leaching solution of waste phosphors by solvent extraction.

10

Separation of Co(II), Cu(II), Ni(II) and Mn(II) from synthetic hydrochloric acid leaching solution of spent lithium ion batteries by solvent extraction

Nguyen Viet Nhan Hoa, Lee Man Seung

Physicochemical Problems of Mineral Processing

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2020

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Vol. 56, iss. 4

699--610

EN

Spent lithium ion batteries contain valuable critical metals such as cobalt, copper, lithium and nickel. In order to develop a process for the separation of the divalent metal ions from spent lithium ion batteries, solvent extraction experiments were performed by employing synthetic hydrochloric acid leaching solution. The synthetic solution contained Cu(II), Co(II), Mn(II) and Ni(II) and its acidity was 3 M HCl. Extraction with Aliquat 336 led to selective extraction of Cu(II) with a small amount of Co(II). After adding NaCl to the Cu(II) free raffinate to enhance the complex formation of Co(II), Co(II) was selectively extracted into Aliquat 336 together with Mn(II). The small amount of Mn(II) in the loaded Aliquat 336 was scrubbed by pure Co(II) solution. After adjusting the pH of the raffinate to 3, 91,3% of Mn(II) was selectively extracted over Ni(II) by the mixture of D2EHPA and Alamine 336. In this extraction, the mole fraction of D2EHPA in the mixture affected the extraction of Mn(II). McCabe-Thiele diagrams for the extraction of Cu(II) and Co(II) were constructed. Batch simulation experiments for the three stage counter-current extraction verified the selective extraction of the target metal ions in each extraction step. Namely, the total extraction percentage of Cu(II) and Co(II) was 71.6% and 98.8% respectively. Most metals in the loaded organic phase were stripped completely with the appropriate agents (1.0 M H2SO4 for Cu(II), 0.1 M H2SO4 for Co(II) and 0.3 M HCl for Mn(II) stripping). A process was proposed to separate the metal ions by solvent extraction.