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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.

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Improvement of leaching efficiency of cathode material of spent LiNixCoy MnzO2 lithium-ion battery by the in-situ thermal reduction

Lu Qichang, Jiang Haidi, Xie Weining, Zhang Guangwen, He Yaqun, Duan Chenlong, Zhang Jing, Yu Zhaoyi

Physicochemical Problems of Mineral Processing

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2021

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Vol. 57, iss. 2

70--82

EN

Green cars and electronic products consume lots of lithium-ion batteries (LIBs), and massive spent LIBs are yielded due to performance degradation. This paper provides an economical and environmentally friendly approach to recover valuable metals from cathode materials of the spent LIBs. It combines the in-situ thermal reduction (self-reduction by polyvinylidene fluoride (PVDF) and residual electrolyte in cathode material) and sulfuric acid leaching. Elements of high valent are reduced by the binder (PVDF) and the residual electrolyte on the surface of NCM(LiNixCoyMn1-x-yyO2) material at high temperatures. Moreover, the changes in substance type, element valency, and contents of cathode materials reduced with various terminal temperatures and retention time are analyzed by Xray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Results show that the optimal terminal temperature for in-situ thermal reduction is 600 °C, and the optimum retention time is 120 min. Under the best in-situ thermal reduction conditions, the results from XRD confirm that part of Ni2+ is converted to simple substance Ni, Co3+ is reduced to Co, and Mn4+ is reduced to Mn2+ and elemental Mn, which are confirmed by XRD. Analyzed results by XPS indicate that the content of Ni2+ decreases to 67.05%, and Co3+ is completely reduced to Co. Mn4+ is reduced to 91.41% of Mn2+ and 8.59% of simple substance Mn. In-situ thermal reduction benefits the leaching processes of cathode materials. The leaching efficiencies of Ni, Co, and Mn increase from 53.39%, 51.95%, and 0.71% to 99.04%, 96.98%, and 97.52%, respectively.

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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.

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Pre-concentration of graphite and LiCoO2 in spent lithium-ion batteries using enhanced gravity concentrator

Zhu X,-N., Tao Y.-J., He Y.-Q., Zhang Y., Sun Q.-X.

Physicochemical Problems of Mineral Processing

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2018

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Vol. 54, iss. 2

293--299

EN

The pre-concentration of electrode material of spent lithium-ion battery has great significance on the resource utilization and environmental protection. The feasibility of separation of graphite and LiCoO2 based on density difference using the enhanced gravity concentrator was verified in this paper. Combustion characteristics of LiCoO2 and graphite were used to propose a simple evaluation index of separation efficiency. Separation tests were carried out to specify the influence of operating parameters on the separation efficiency. Moreover, the effect of particle size on the separation performance was studied. Combustion characteristics results showed that mass loss of graphite was much greater than that of LiCoO2. Thus, mass loss were used to evaluate the purity of product. Effective separation of graphite and LiCoO2 was achieved by the enhanced centrifugal separator. Separation results showed that increasing centrifugal force decreased the overflow yield and increased the graphite content of the overflow stream. In addition, yield of overflow grew an increase in fluidization water pressure, while the purity of graphite in overflow decreased. The effect of particle size on the separation efficiency was also significant, the separation efficiency decreased with the decreasing of particle size.

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Przerób zużytych baterii litowo-jonowych (Li-jon) w Polsce

Sobianowska-Turek A., Wasiewska S., Wierzbicka W.

Przemysł Chemiczny

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2016

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T. 95, nr 9

1815--1821

PL

Przedstawiono podstawy formalnoprawne oraz analizę ilościowo-jakościową zużytych baterii litowo-jonowych w Polsce w latach 2010–2014 oraz szacunkowe ich ilości na rynku do 2020 r. Dodatkowo zaprezentowano światowe technologie recyklingu oraz polskie procesy, w których przetwarzane są chemiczne źródła energii.

EN

Legal regulations concerning management of Li-ion battery waste in Poland as well as statistical data for future Li-ion waste stream up to 2020 were given. A review of recycling technols. was also included.

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Metal Bioleaching from Spent Lithium-Ion Batteries Using Acidophilic Bacterial Strains

Marcincakova R., Kadukova J., Mrazikova A., Velgosova O., Luptakova A., Ubaldini S.

Inżynieria Mineralna

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2016

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R. 17, nr 1

117--120

EN

In this present work lithium and cobalt recovery from spent lithium-ion batteries (27.5% LiCoO2) by bioleaching was investigated. The experiments were carried out using the consortia of acidophilic bacteria of Acidithiobacillus ferrooxidans and Acidithiobacillus thiooxidans. For the Li and Co bioleaching two different media were used. A rich nutrient medium was consisted of all minerals needed for bacterial growths, whereas a low nutrient medium contained only sulphuric acid and elemental sulphur as an energy source. In the rich nutrient medium the overall lithium and cobalt bioleaching efficiency was 80% and 67%, respectively, whereas in the low nutrient environment only 35% Li and 10.5% Co were released. The experimental results revealed that the presence of nutrients in the bioleaching medium influenced, to a large extent, lithium and cobalt dissolution from LIBs.

PL

W prezentowanym artykule zbadano odzysk litu i kobaltu ze zużytych baterii litowo-jonowych (27.5% LiCoO2) za pomocą bioługowania. Eksperymenty zostały przeprowadzone za pomocą kultur bakterii kwasolubnych Acidithiobacillus ferrooxidans oraz Acidithiobacillus thiooxidans. Dla bioługowania Li i Co zastosowano dwa różne ośrodki: ośrodek bogaty we wszystkie minerały potrzebne do wzrostu bakterii oraz ośrodek o niskiej zawartości substancji odżywczych, którym był ośrodek zawierający jedynie kwas siarkowy oraz siarkę pierwiastkową jako źródło energii. W pierwszym ośrodku ogólna efektywność bioługowania litu i kobaltu wyniosła, odpowiednio, 80% i 67%. Dla drugiego ośrodka wyniki te były, odpowiednio, 35% Li oraz 10.5% Co. Wyniki eksperymentalne ukazały, że obecność substancji odżywczych w bioługowaniu wpływa znacząco na odzyskanie litu i kobaltu z baterii litowo-jonowych.