Preparation of High-Purity Lithium Carbonate Using Complexing Ion-Exchange Resins

Milyutin, V. V.; Некрасова, Н. А.; Рудских, В. В.; Волкова, Т. С.

doi:10.1134/s1070427220040096

Cited by 7 publications

(7 citation statements)

References 4 publications

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“…Lithium has traditionally been used in a variety of applications ranging from pharmaceuticals to the manufacture of air treatment systems . The main sources to extract lithium are ores (spodumene, lepidolite, petalite, among others), brines, and mineral groundwater . Due to its low atomic mass, Li has a high charge, and the power to weight ratio enables it to store and transmit energy, making in an important component for the construction of rechargeable lithium-ion batteries (LIBs) .…”

Section: Introductionmentioning

confidence: 99%

“… 1 The main sources to extract lithium are ores (spodumene, lepidolite, petalite, among others), brines, and mineral groundwater. 2 Due to its low atomic mass, Li has a high charge, and the power to weight ratio enables it to store and transmit energy, making in an important component for the construction of rechargeable lithium-ion batteries (LIBs). 1 With their high energy density, low self-discharge rate, and high open-circuit voltage, LIBs can be widely used in electronic devices, as well as in hybrid electric vehicles (HEVs) and electric vehicles (EV).…”

Section: Introductionmentioning

confidence: 99%

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Analysis of Trace Impurities in Lithium Carbonate

Suárez,

Jara,

Castillo

et al. 2024

ACS Omega

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Lithium carbonate (Li 2 CO 3 ) is a critical raw material in cathode material production, a core of Li-ion battery manufacturing. The quality of this material significantly influences its market value, with impurities potentially affecting Li-ion battery performance and longevity. While the importance of impurity analysis is acknowledged by suppliers and manufacturers of battery materials, reports on elemental analysis of trace impurities in Li 2 CO 3 salt are scarce. This study aims to establish and validate an analytical methodology for detecting and quantifying trace impurities in Li 2 CO 3 salt. Various analytical techniques, including X-ray diffraction (XRD), scanning electron microscopy− energy-dispersive X-ray spectroscopy (SEM-EDX), X-ray photoelectron spectroscopy (XPS), and inductively coupled plasma optical emission spectroscopy (ICP-OES), were employed to analyze synthetic and processed lithium salt. Xray diffraction patterns of Li 2 CO 3 were collected via step-scanning mode in the 5−80°2θ range. SEM-EDX was utilized for particle morphology and quantitative impurity analysis, with samples localized on copper tape. XPS equipped with a hemispherical electron analyzer was employed to analyze the surface composition of the salt. For ICP-OES analysis, a known amount of lithium salt was subjected to acid digestion and dilution with ultrapure water. Multielemental standard solutions were prepared, including elements such as Al, Cd, Cu, Fe, Mn, Ni, Pb, Si, Zn, Ca, K, Mg, Na, and S. Results confirmed the presence of the zabuyelite phase in XRD analysis, corresponding to the natural form of lithium carbonate. SEM-EDX mapping revealed impurities of Si and Al, with low relative quantification values of 0.12% and 0.14%, respectively. XPS identified eight potential impurity elements, including S, Cr, Fe, Cl, F, Zn, Mg, and Na, alongside Li, O, and C. Regarding ICP-OES analysis, performance parameters such as linearity, limit of detection (LOD), and quantification (LOQ), variance, and recovery were evaluated for analytical validation. ICP-OES results demonstrated high linearity (>0.99), with LOD and LOQ values ranging from 0.001 to 0.800 ppm and 0.003 to 1.1 ppm, respectively, for different elements. The recovery rate exceeded 90%. In conclusion, the precision of the new ICP-OES methodology renders it suitable for identifying and characterizing Li 2 CO 3 impurities. It can effectively complement solid-state techniques such as XRD, SEM-EDX, and XPS.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Analysis of Trace Impurities in Lithium Carbonate

Suárez,

Jara,

Castillo

et al. 2024

ACS Omega

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“…The sorption method is a more attractive and easy-to-manage process that does not require additional chemicals. Milutin and coauthors used chelating commercial sorbents, such as Purolite S930, Amberlite IRC 748, and AXIONIT 3S, and obtained results demonstrating that lithium salts (Li 2 CO 3 and LiCl) of high purity could be obtained [ 12 ]. These sorbents manifested selectivity toward certain transition metals and their combination yielded a purification level of 99.90%.…”

Section: Introductionmentioning

confidence: 99%

Investigation on Purification of Saturated LiNO3 Solution Using Titanium Phosphate Ion Exchanger: Kinetics Study

Маслова

Иваненко

Evstropova

et al. 2022

IJMS

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Lithium compounds are of high interest to many industries. The presence of undesirable impurities in Li precursors leads to uncontrolled change in the functional properties of final compounds. Therefore, the development of reliable methods for lithium salt purification is considered a key factor for their application in various industries. This work focuses on the application of a titanium phosphate ion exchanger (Li-TiOP) toward Cu2+, Co2+, Mn2+, Ni2+, and Cr3+ ions in the purification of a saturated LiNO3 solution. The sorption kinetics of the selected ions, considering external and internal mass transfer, as well as chemical interaction, were deeply studied. The kinetic study showed that the values of intraparticle diffusion rate and effective diffusion coefficients for the studied ions decreased in the following order: Cr(III) Cu(II) Mn(II) ˃ Co(II) ˃ Ni(II). For all the selected ions, chemical interaction was described with a pseudo-second-order reaction model. The sorption kinetics were controlled by the size of the solvated metal ion, its effective charge, the electronic structure of the adsorbed ion, and the interaction with the functional groups of the sorbent. Due to fast kinetics, the high degree of removal of trace quantities of the impurities this material gives it consideration as a promising sorbent for the deep purification of lithium salts.

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“…Meanwhile, the influencing factors of Li 2 CO 3 crystallization are also investigated. [27][28][29] It is worth noting that these studies mainly focus on reducing impurities contents and obtaining high purity Li 2 CO 3 . Therefore, regardless of which approach you choose, impurities contents in the final product must be controlled seriously, because the pureness of Li 2 CO 3 can directly affect the usage in LIBs.…”

Section: Introductionmentioning

confidence: 99%

Preparation of Battery Grade Li₂CO₃ from Defective Product by the Carbonation‐Decomposition Method

Zhou¹

2022

Cryst. Res. Technol.

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Battery grade Li 2 CO 3 is successfully synthesized by the carbonation-decomposition method using defective crude Li 2 CO 3 with the purity of 98.56 wt% containing 5873 ppm SO 4 2− and other impurities such as Na, K, Ca, Fe, and Mg. Filter operation is found to be very important to improve quality of products. The purified Li 2 CO 3 precipitation acquired by filtering the LiHCO 3 solution possesses a higher purity of 99.65 wt% and greater whiteness with lower amounts of SO 4 2− (222.0 ppm) and Fe (6.6 ppm). For further purification, ethylenediaminetetraacetic acid disodium salt is added into the LiHCO 3 solution then Ca and Fe contents in purified Li 2 CO 3 are reduced to 2.9 and 0.7 ppm, respectively. The removal efficiencies obtained for Ca, Fe, and SO 4 2− are of 80.05%, 99.4%, and 97.5%, respectively. The research of reaction kinetics shows that the rate-determining step of the carbonation process is diffusion control and the generated HCO 3 − ions can resist the further dissolution of CO 2 . The theoretical thermal decomposition temperature is 277.10 K by the thermodynamic calculation. SO 4 2− impurity comes from absorbed Na 2 SO 4 and doped Li 2 SO 4 . This work is of great significance to economically and simply treat defective product with high impurity content in the actual Li 2 CO 3 production process.

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Preparation of High-Purity Lithium Carbonate Using Complexing Ion-Exchange Resins

Cited by 7 publications

References 4 publications

Analysis of Trace Impurities in Lithium Carbonate

Analysis of Trace Impurities in Lithium Carbonate

Investigation on Purification of Saturated LiNO3 Solution Using Titanium Phosphate Ion Exchanger: Kinetics Study

Preparation of Battery Grade Li₂CO₃ from Defective Product by the Carbonation‐Decomposition Method

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Preparation of High-Purity Lithium Carbonate Using Complexing Ion-Exchange Resins

Cited by 7 publications

References 4 publications

Analysis of Trace Impurities in Lithium Carbonate

Analysis of Trace Impurities in Lithium Carbonate

Investigation on Purification of Saturated LiNO3 Solution Using Titanium Phosphate Ion Exchanger: Kinetics Study

Preparation of Battery Grade Li2CO3 from Defective Product by the Carbonation‐Decomposition Method

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Product

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Preparation of Battery Grade Li₂CO₃ from Defective Product by the Carbonation‐Decomposition Method