Preparation of Battery-Grade Lithium Carbonate with Lithium-Containing Desorption Solution - MDPI
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metals Article Preparation of Battery-Grade Lithium Carbonate with Lithium-Containing Desorption Solution Zheng-Guo Xu 1 and Shu-Ying Sun 1,2, * 1 National Engineering Research Center for Integrated Utilization of Salt Lake Resource, School of Resources and Environmental Engineering, East China University of Science and Technology, Shanghai 200237, China; xzgetl@163.com 2 Joint International Laboratory for Potassium and Lithium Strategic Resources, School of Resources and Environmental Engineering, East China University of Science and Technology, Shanghai 200237, China * Correspondence: shysun@ecust.edu.cn Abstract: In this study, a process for preparing battery-grade lithium carbonate with lithium-rich solution obtained from the low lithium leaching solution of fly ash by adsorption method was proposed. A carbonization-decomposition process was carried out to remove impurities such as iron and aluminum. First, primary Li2 CO3 was treated by CO2 to get the more soluble bicarbonates. The decomposition of LiHCO3 produced insoluble Li2 CO3 at 90 ◦ C And Li2 CO3 was smashed by air stream pulverization. The final precipitation yielded a high purity (99.6%) and homogeneous Li2 CO3 . Some factors affecting production efficiency were investigated. The results showed that a liquid-solid ratio of 25:1, a carbonization temperature of 25 ◦ C, an air velocity of 2 L/min, and a stirring speed of 400 rpm; a decomposition temperature of 90 ◦ C and a stirring speed of 400 rpm, a molar ratio of EDTA to Ca 2:1; an air pressure of 0.3 MPa and hot water washing precipitate (L/S mass ratio 2:1) promoted ions removal. Citation: Xu, Z.-G.; Sun, S.-Y. Preparation of Battery-Grade Lithium Keywords: lithium carbonate; carbonation; decomposition; battery-grade; air stream pulverization Carbonate with Lithium-Containing Desorption Solution. Metals 2021, 11, 1490. https://doi.org/10.3390/ met11091490 1. Introduction Lithium has become one of the most significant resources around the world due to the Academic Editors: Rahul Ram and fast-growing lithium-ion battery demand nowadays. Lithium carbonate is used in many Mark I. Pownceby industries as the initial raw material. Especially in the field of new energy, battery-grade lithium carbonate is required, which has higher requirements for the lithium carbonate Received: 4 August 2021 process. Accepted: 17 September 2021 At present, the preparation of lithium carbonate from salt lake brine is usually by Published: 19 September 2021 the evaporation-crystallization-precipitation method. Among that the development of carbonate precipitation is relatively mature and is suitable for brines with a low Mg/Li Publisher’s Note: MDPI stays neutral ratio. Various additives (such as sodium bicarbonate and oxalic acid [1,2]), ultrasonic with regard to jurisdictional claims in published maps and institutional affil- waves [3], and reaction systems [4,5] were studied to discuss the influence on crystal iations. size and morphology. Sun [6] made a systematic study on the crystallization process of lithium carbonate and prepared lithium carbonate products with various purity, granularity, and morphology. Three industrial routes of Li2 CO3 recrystallization, LiHCO3 thermal decomposition reaction crystallization, and LiOH + CO2 gas-liquid crystallization were used to prepare high-purity lithium carbonate products with purity higher than 99.9%. Copyright: © 2021 by the authors. The industrial production of battery-grade lithium carbonate generally does not Licensee MDPI, Basel, Switzerland. directly carry out from ore and brine, because these principles contain high impurities thus This article is an open access article distributed under the terms and it is difficult to guaranteed purity [7–10]. Therefore, industrial-grade lithium carbonate is conditions of the Creative Commons obtained from different lithium resources through different separation processes and then Attribution (CC BY) license (https:// purified to obtain battery-grade lithium carbonate [11–13]. Carbonization is one of the more creativecommons.org/licenses/by/ commonly used methods which mainly reacts lithium carbonate with carbon dioxide and 4.0/). water to generate lithium bicarbonate with greater solubility [14]. Generally, ion-exchanged Metals 2021, 11, 1490. https://doi.org/10.3390/met11091490 https://www.mdpi.com/journal/metals
Metals 2021, 11, 1490 2 of 10 resin is used to remove calcium and magnesium impurities with the inevitable loss of lithium [15]. In recent years, with the development of high-value added utilization of solid waste, the recovery of lithium, gallium, and other elements in fly ash has been on the agenda. In previous studies, we proposed a method of extracting lithium from fly ash with a lithium content of 0.25 mg/g and obtained a lithium-containing desorption solution [16]. This research was based on the solution to design a battery-grade lithium carbonate process. It was realized that fly-ash was another high-value source for lithium extraction. Compared with traditional technologies, iron, aluminum, and silicon can be removed effectively from lithium carbonate using this method. Meanwhile, the resin adsorption process of impurity ions can be eliminated. The strategy is effective to control product granularity to meet the requirements of battery-grade lithium carbonate. The effects of various factors on the yield and purity of the final lithium carbonate product were investigated, and a set of feasible process schemes were provided. 2. Methods 2.1. Materials and Chemicals Lithium-containing desorption solution was obtained from the low lithium leaching solution of fly ash by the adsorption method [16] with a concentration shown in Table 1. The main impurity ions in the desorption solution are sodium, iron, aluminum, and silicon. The concentration of lithium is about 13.59 g/L. All chemicals in the study were analytical grade. Table 1. Main compositions of the lithium-containing desorption solution. Li Na Al K Ca Fe g/L 13.59 70.04 0.0328 1.006 0.3172 0.0366 2.2. Experimental Equipment and Analytical Instruments A constant temperature water bath, a DZF-6090 vacuum drying oven, an AR2140 OHAUS precision analytical balance, an S10-3 constant temperature magnetic stirrer, a PHSJ-3F laboratory pH meter, an ARCOS FHS12 inductively coupled plasma emission spectrometer, a MASTERSIZER 2000 laser particle size instrument (Malvern Instruments Ltd, Malvern, UK), and an S-3400N Scanning Electron Microscope (Hitachi Corporation of Japan, Tokyo, Japan) were used in this study. 2.3. Methods Figure 1 outlined the major steps involved in the production of battery-grade Li2 CO3 . The lithium-containing desorption solution was concentrated first, and the saturated sodium carbonate solution was added to obtain a primary lithium carbonate product with purity as shown in Table 2. The optimal reaction conditions were reported by recent research [17]: a reaction temperature of 90 ◦ C, the dosage of sodium carbonate was 1.1 times the theoretical reaction dosage, a feed rate of 17 mL/min, and a stirring rate of 200 rpm. Hot water (90 ◦ C) and ethanol were used to remove sodium ions. Second, at different temperatures (25, 30, 35, 40, 45 ◦ C), the primary lithium carbonate product was soaked in water with a liquid-solid ratio (10, 20, 30, 40, 50), then CO2 (99%) was bubbled into the slurry with different flow rate (1.0, 1.5, 2.0, 2.5, 3.0 L/min). And the Li2 CO3 was converted to soluble LiHCO3 . The lithium bicarbonate solution was obtained by filtration. Finally, the lithium bicarbonate solution was added to the reactor and heated at a constant temperature (60, 70, 80, 90 ◦ C) in a water bath. After the reaction, the solids were washed twice with hot water and dried in an oven. Then the air stream pulverization was used to treat the high purity lithium carbonate.
Metals 2021, Metals 11, x1490 2021, 11, FOR PEER REVIEW 3 3ofof 11 10 Figure Figure1.1.Flowsheet Flowsheetdeveloped developedfor forthe therecovery recoveryof ofbattery-grade battery-grade Li Li22CO CO33from fromthe thelithium-containing lithium-containing desorption solution. desorption solution. Table Table 2. 2. Impurity Impurity content content of of primary primary lithium lithium carbonate carbonate products. products. Li 2CO3 Li2 CO3 Na Na Al Al K K Ca Ca Fe Fe 92.21% 4.213% 0.019% 0.049% 0.411% 0.042% 92.21% 4.213% 0.019% 0.049% 0.411% 0.042% Second, at different temperatures (25, 30, 35, 40, 45 °C), the primary lithium carbonate 3. Results product wasand Discussion soaked in water with a liquid-solid ratio (10, 20, 30, 40, 50), then CO2 (99%) 3.1. Washing Process of was bubbled into the slurry Products with different flow rate (1.0, 1.5, 2.0, 2.5, 3.0 L/min). And the Li2COSpecial attention to 3 was converted was paid LiHCO soluble to the effect 3. Theof the washing lithium process, bicarbonate and the solution wasresults are obtained shown by in Figure 2. The washing process mainly removes sodium from the product. Water filtration. has aFinally, higher impurity removal the lithium efficiency bicarbonate than ethanol, solution but attothe was added same the time,and reactor the heated lithium at loss a is higher. It can be due to the lithium carbonate is more soluble in water than ethanol. constant temperature (60, 70, 80, 90 °C) in a water bath. After the reaction, the solids were When using water washed twiceaswith a detergent, hot watertheandcontent dried of in impurities did the an oven. Then not air change significantly stream withwas pulverization the increase in washing times. But at the same time, the lithium loss increased continuously. It used to treat the high purity lithium carbonate. can be seen that there was a sudden increase in sodium after the fourth washing. It might beResults 3. due to the andimpurities Discussion that have been removed completely while lithium carbonate was still being lost. 3.1. Washing Process of Products Special attention was paid to the effect of the washing process, and the results are shown in Figure 2. The washing process mainly removes sodium from the product. Water has a higher impurity removal efficiency than ethanol, but at the same time, the lithium loss is higher. It can be due to the lithium carbonate is more soluble in water than ethanol.
When using water as a detergent, the content of impurities did not change significantly with the increase in washing times. But at the same time, the lithium loss increased con- tinuously. It can be seen that there was a sudden increase in sodium after the fourth wash- Metals 2021, 11, 1490 ing. It might be due to the impurities that have been removed completely while lithium4 of 10 carbonate was still being lost. Figure 2. Washing process of water and ethanol: (a) lithium loss; (b) sodium content. Figure 2. Washing process of water and ethanol: (a) lithium loss; (b) sodium content. 3.2. Conversion of 3.2. Conversion of Impurities Impurities during during Carbonization Carbonization Process Process The The concentration of impurities in the solution after concentration of impurities in the solution after carbonization carbonization was was measured measured as as shown shown in Figure 3. It can be seen that the concentration of impurities in the solutiongener- in Figure 3. It can be seen that the concentration of impurities in the solution gen- ally increased erally increasedfirst and first then and decreased then decreasedwith time. with TheThe time. change changeof calcium ionion of calcium concentration concentra- was particularly obvious, which may be due to calcium carbonate tion was particularly obvious, which may be due to calcium carbonate and lithiumand lithium carbonate car- have the same properties and react with carbon dioxide. And calcium bonate have the same properties and react with carbon dioxide. And calcium bicarbonate bicarbonate is easy to decompose at room temperature, resulting in a precipitation reaction. is easy to decompose at room temperature, resulting in a precipitation reaction. However, However, Fe CO33 and Fe22CO and Al Al22CO CO33did didnot notreact react with with carbon carbon dioxide dioxide atat experimental experimental temperatures. temperatures. The The impurities dissolve slightly during the process of slurring. But the precipitation reaction impurities Metals 2021, 11, x FOR PEER dissolve REVIEW slightly during the process of slurring. But the precipitation 3+ and Al3+ occurs with the decrease of pH from 12 to 7 during the carbonization reaction of Fe3+ of Fe and Al3+ occurs with the decrease of pH from 12 to 7 during the carbonization pro- process [5]. cess [5]. Figure 3. Effect of L/S Figure (a) temperature 3. Effect (b) flow rate(b) of L/S (a) temperature (c) flow time rate (d) on (c)the concentration time of impuritiesof[liquid-solid (d) on the concentration impurities ratio = 20 temperature[liquid-solid = 25 °C, flow rate of CO = 3 L/min]. ◦ ratio = 20, temperature = 25 C, flow rate of CO2 = 3 L/min]. 2 3.3. Optimization of Carbonization Process In this study, the liquid-solid ratio (mL/g) refers to the ratio of the volume of d ized water and the mass of solid lithium carbonate. The effects of different liquid ratios on carbonization reaction rates were studied. The conversion rate could be
Metals 2021, 11, 1490 5 of 10 3.3. Optimization of Carbonization Process In this study, the liquid-solid ratio (mL/g) refers to the ratio of the volume of deionized water and the mass of solid lithium carbonate. The effects of different liquid-solid ratios on carbonization reaction rates were studied. The conversion rate could be calculated as follows: CV/13.88 × 73.89 ϕ= × 100% (1) W where C is the concentration of Li+ in the solution (mg/L), V is the volume of the solution (L), W is the Initial mass of lithium carbonate (mg). As can be seen from Figure 4, the conversion rate of lithium carbonate increased as the liquid-solid ratio increased. It can be explained that with an increase in the liquid-solid ratio, the bulk concentration of the slurry mixture decreased, which reduces the diffusion resistance in the liquid phase and at the liquid-solid boundary. On the other hand, as the solid concentration decreased, the slurry density and the friction between phases decreased, so that the total interface area of the reaction and the mass transfer rate increased [11]. The more fully lithium carbonate is in contact with carbon dioxide, the faster the reaction Metals 2021, 11, x FOR PEER REVIEWrate will be. As can be seen, the conversion rate was only 40% at a liquid-solid ratio 6 of of 11 10 mL/g. It might be that the solubility limit of lithium bicarbonate in an aqueous solution was reached, and the reaction could not proceed anymore. Figure 4. Effect Effectof ofliquid-solid liquid-solidratio ratioonon carbonization reaction carbonization [temperature reaction 25 ◦flow = 25= °C, [temperature rate rate C, flow of COof2 = 3 2L/min]. CO = 3 L/min]. The conversion conversion raterateof oflithium lithiumcarbonate carbonateatatdifferent differenttemperatures temperatures is is shown showninin Figure Figure5. The carbonization 5. The carbonization process process is iscontrolled controlledbybymass masstransfer transferand andreaction, reaction, inin which which mass mass transfer is the main control control process process [18]. [18]. The dissolution dissolution rates ofof lithium lithium carbonate carbonate and and carbon dioxide decreased with the increase in temperature, resulting in the decrease decrease of of mass transfer transfer efficiency efficiency and and the theincrease increaseininreaction reactionrate. rate.OnOn the other hand, the other hand, lithium lithiumbi- bicarbonate carbonate willwillbebedecomposed decomposedatathigh hightemperatures. temperatures.Thus,Thus,as asthe thetemperature temperature increased, increased, the the concentration concentration of of lithium lithium at at the the reaction reaction endpoint endpoint decreased, decreased, which which means means that that the the conversion rate gradually decreases. conversion rate gradually decreases.
5. The carbonization process is controlled by mass transfer and reaction, in which mass transfer is the main control process [18]. The dissolution rates of lithium carbonate and carbon dioxide decreased with the increase in temperature, resulting in the decrease of mass transfer efficiency and the increase in reaction rate. On the other hand, lithium bi- carbonate will be decomposed at high temperatures. Thus, as the temperature increased, Metals 2021, 11, 1490 6 of 10 the concentration of lithium at the reaction endpoint decreased, which means that the conversion rate gradually decreases. Effect Figure5.5.Effect Figure of temperature of temperature on carbonization on carbonization reaction reaction [liquid-solid [liquid-solid ratio ratio = 20,rate = 20, flow flowof rate CO2 of = CO = 3 3 L/min]. 2 L/min]. Ascan As canbebeseen seenfrom fromFigure Figure6,6,with withincreasing increasingthe theflow flowrate rate of of CO CO22, ,the thecarbonation carbonation reaction rate was accelerated. It might be due to the volume mass reaction rate was accelerated. It might be due to the volume mass transfer coefficient transfer coefficient in- increased with the increase in creased with the increase in CO2 flow Metals 2021, 11, x FOR PEER REVIEW CO 2 flow rate. Similarly, these results were consistent rate. Similarly, these results were consistent7 with with of 11 moststudies most studiesininthat thatusing usingaahighhighflow flow rate rate can can enhance enhance Li Li22CO CO33dissolution dissolutionin inCO CO22–water –water solution [19]. However, it is not difficult to find that, with the increase solution [19]. However, it is not difficult to find that, with the increase in CO in CO flow rate, 2 2 flow rate, the ventilation the volume ventilation volume increased increasedsignificantly within significantly withinthe the same period, same but but period, the theutilization rate utilization rate of2CO of CO 2 decreased decreased relative relative to volume. to the the volume. Thus,Thus, it is appropriate it is not not appropriate to use toanuseexcessively an exces- sively highrate high flow flowinrate in industrial industrial applications, applications, and a and a previous previous studystudy reported reported that increas- that increasing the ing the pressure may improve the effective utilization pressure may improve the effective utilization rate of CO2 . rate of CO 2 . Figure Figure6.6.Effect Effectof offlow flowrate rateon oncarbonization carbonization reaction reaction [liquid-solid [liquid-solid ratio ratio == 20, 20, temperature temperature ==25 ◦ C]. 25°C]. The pH The pH of the the reaction reactionsystem systematatdifferent different time timeintervals intervals was shown was in Figure shown 7. It 7. in Figure wasIt noticed was that that noticed during the carbonation during process the carbonation the pH process theofpHtheofsolution started the solution at about started 11.85 at about and reached 11.85 aboutabout and reached 7.5 in7.5 theinend, theitend, can itbecan seen bethat seenthe acidity that of the of the acidity solution increased the solution in- during carbonation. creased Finally, Finally, during carbonation. all Li2 CO was all3 Li 2COconverted to soluble 3 was converted LiHCO3LiHCO to soluble . Therefore, the 3. There- progress fore, of the reaction the progress can be accounted of the reaction for by thefor can be accounted variation of pH. of pH. by the variation
The pH of the reaction system at different time intervals was shown in Figure 7. It was noticed that during the carbonation process the pH of the solution started at about 11.85 and reached about 7.5 in the end, it can be seen that the acidity of the solution in- Metals 2021, 11, 1490 7 of 10 creased during carbonation. Finally, all Li2CO3 was converted to soluble LiHCO3. There- fore, the progress of the reaction can be accounted for by the variation of pH. Figure Figure7.7.Variation Variationof ofpH pHas asaafunction functionof oftime. time. 3.4.The 3.4. TheEffect EffectofofDecomposition DecompositionConditions ConditionsononProducts Products Asisisshown showninin Figures 8 and 9, 9, when the ◦ C to As Figure 8 and Figure when thetemperature temperatureincreased increasedfrom from 60 60 °C to 90 ◦ C, the reaction rate and conversion rate of LiHCO increased significantly [19,20]. 90 °C, the reaction rate and conversion rate of LiHCO3 increased significantly [19,20]. The Metals 2021, 11, x FOR PEER REVIEW 3 8 of 11 The decomposition process of the LiHCO solution is an endothermic reaction, decomposition process of the LiHCO3 solution is an endothermic reaction, so its equilib- 3 so its equilibrium rium is shiftedistoshifted to the side the product product with side with increasing increasing temperatures temperatures andthe and promotes promotes solute the solute diffusion and crystal growth rate. In conclusion, it is beneficial for both the diffusion and crystal decomposition growth and of LiHCO rate.the In conclusion, it is beneficial crystallization of Li2 CO3for toboth the decomposition increase the operating 3 of LiHCO temperature. 3 and the crystallization of Li2CO3 to increase the operating temperature. Figure Figure 8. Effect of 8. Effect oftemperature temperatureonon thermal thermal decomposition decomposition crystallization crystallization [agitation [agitation speedspeed = 300 =rpm]. 300 rpm]. Figure 9. Sem-analysis of products under different temperatures. Agitation speed is also one of the factors that affect thermal decomposition reaction. The particle size distribution of the products under different agitation speeds was inves- tigated as shown in Figure 10. It can be seen that with the increase in agitation speed, the
Metals 2021, 11, 1490 8 of 10 Figure 8. Effect of temperature on thermal decomposition crystallization [agitation speed = 300 rpm]. Figure 9. Figure 9. Sem-analysis Sem-analysis of of products products under under different different temperatures. temperatures. Agitation speed is also one of the factors that affect thermal decomposition reaction. The particle size distribution of the products under different agitation speeds was inves- tigated as as shown shown in inFigure Figure10.10.It Itcan canbebeseen that seen with that thethe with increase in agitation increase speed, in agitation the speed, single the crystal single peak crystal shifts peak to the shifts left,left, to the andandthethe height of of height thethe coalescence coalescencepeak peakincreased. increased. It can It bebe can explained explained that with that thethe with increase increasein in agitation speed, agitation both speed, thethe both liquid turbulence liquid turbulence in- Metals 2021, 11, x FOR PEER REVIEWintensity tensity andandthethe interface interface updating updating speed speed werewere increased. increased. It conducive It was was conducive to thetodiffusion the 9 ofdif- 11 fusion of lithium of lithium carbonate carbonate solute andsolute theand the growth growth of surface of crystal crystal surface and improving and improving the the crystal- crystal-crushing crushing effect ateffect at thetime. the same same time. Effect of of agitation agitation speed speed on on thermal thermal decomposition ◦ Figure 10. Figure 10. Effect decomposition crystallization crystallization [temperature [temperature== 90 90 C]. °C]. It is difficult to make the product directly meet the particle size requirement of battery- gradeItlithium carbonate is difficult to makeby the stirring and seed product addition. directly In this meet the paper,size particle airstream pulverization requirement of bat- was used to treat the product. The pulverizing effect of the jet mill under tery-grade lithium carbonate by stirring and seed addition. In this paper, airstream differentpul- air compressor verization waspressures used to was treatstudied as shown the product. in Figure 11.effect The pulverizing Theof average the jet particle mill undersizedif- of the product decreased with the increase in air compressor pressure. The jet ferent air compressor pressures was studied as shown in Figure 11. The average particle mill ejects the compressed size gas at adecreased of the product high speed through with the nozzle. the increase The in air high-speed compressor airflow brought pressure. the The jet mill material to the crushing chamber where the particles were crushed by collision, friction, ejects the compressed gas at a high speed through the nozzle. The high-speed airflow and shear. The air compressor pressure affects the air velocity, which affects the impact brought the material to the crushing chamber where the particles were crushed by colli- strength of the particles, and the product with different particle size distribution was sion, friction, and shear. The air compressor pressure affects the air velocity, which affects obtained. the impact strength of the particles, and the product with different particle size distribu- tion was obtained.
ejects the compressed gas at a high speed through the nozzle. The high-speed airflow brought the material to the crushing chamber where the particles were crushed by colli- sion, friction, and shear. The air compressor pressure affects the air velocity, which affects the impact strength of the particles, and the product with different particle size distribu- Metals 2021, 11, 1490 tion was obtained. 9 of 10 (a) (b) Figure Figure 11. Effect of 11. Effect pressure of pressure on particle onaverage size. (a) particleparticle size. (a)size average particlesize (b) particle size (b) particle size distribution distribution. 4. Conclusions A carbonization-decomposition process was developed to produce battery-grade Li2 CO3 from a lithium-containing desorption solution. The best reaction conditions were obtained: a liquid-solid ratio of 25:1, a carbonization temperature of 25 ◦ C, an air velocity of 2 L/min, a carbonization time of 2 h, and a stirring speed of 400 rpm. And the product finally reaches the battery-grade lithium carbonate battery-grade standard by air-jet crush- ing. The lithium content of the lithium carbonate product obtained through the three-step reaction reaches 99.6%, the content of iron and aluminum in the product is less than 0.001%, contents of other impurities are below the battery-grade lithium carbonate standard, the total yield of the product is about 70%. The particle size of the lithium carbonate product can be controlled by changing the pressure of the jet mill to achieve the battery-grade standard requirement. The entire process has great industrial potential. Author Contributions: Literature search, figures, study design, data collection, data analysis, and writing—original draft preparation and review, Z.-G.X.; methodology, data analysis, and writing—review and editing, S.-Y.S. All authors read and approved the final manuscript. Funding: This research was funded by the National Key R&D Program of China (2017YFB0603104), and Sponsored by Shanghai Pujiang Program (2019PJD011). Institutional Review Board Statement: Not applicable. Informed Consent Statement: Not applicable. Data Availability Statement: Not applicable. Acknowledgments: The research was supported by the National Key R&D Program of China (2017YFB0603104), and Sponsored by the Shanghai Pujiang Program (2019PJD011). Conflicts of Interest: The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, or in the decision to publish the results. References 1. Watamura, H.; Marukawa, H.; Hirasawa, I. Polyelectrolyte effects on the crystallization phenomena of the lithium carbonate. Cryst. Growth 2013, 373, 111–117. [CrossRef] 2. Zhao, C.; Zhang, Y.; Cao, H.; Zheng, X.; Van Gerven, T.; Hu, Y.; Sun, Z. Lithium carbonate recovery from lithium-containing solution by ultrasound assisted precipitation. Ultrason. Sonochem. 2018, 52, 484–492. [CrossRef] [PubMed] 3. Tian, M.; Wang, Z.; Cao, J.; Guo, J.; Gong, X. Insight into Lithium Carbonate Crystallization in the Mild Reaction System LiCl-NH3 ·H2 O-CO2 by Stabilizing the solution with NH3 ·H2 O. Cryst. Growth 2019, 520, 46–55. [CrossRef] 4. Tian, M.; Guo, J.; Wang, Z.; Cao, J.; Gong, X. Synergetic effect of secondary nucleation and growth on the lithium carbonate particle size in the gas–liquid reactive crystallization of LiCl–NH3 ·H2 O–CO2 . Particuology 2020, 51, 10–17. [CrossRef]
Metals 2021, 11, 1490 10 of 10 5. Yi, W.T.; Yan, C.Y.; Ma, P.H.; Wen, X.M. Refining of crude Li2 CO3 via slurry phase dissolution using CO2 . Sep. Purif. Technol. 2007, 56, 241–248. [CrossRef] 6. Sun, Y.; Song, X.; Jin, W.; Yan, L.; Yu, J. Unseeded Supersolubility of Lithium Carbonate: Experimental Measurement and Simulation with Mathematical Models. Cryst. Growth 2009, 311, 4714–4719. [CrossRef] 7. Pan, X.; Dou, Z.H.; Zhang, T.A.; Meng, D.L.; Han, X.X. Basic study on direct preparation of lithium carbonate powders by membrane electrolysis. Hydrometallurgy 2020, 191, 105193. [CrossRef] 8. Yang, W.; Zhou, L.; Dai, J.; Zhou, L.; Yin, Q. Crystallization of Lithium Carbonate from Aqueous Solution: New Insights into Crystal Agglomeration. Ind. Eng. Chem. Res. 2019, 58, 18448–18455. [CrossRef] 9. Wang, W.; Chen, W.; Liu, H. Hydrometallurgical preparation of lithium carbonate from lithium-rich electrolyte. Hydrometallurgy 2019, 185, 88–92. [CrossRef] 10. Han, B.; Louhi-Kultanen, M. Lithium carbonate precipitation by homogeneous and heterogeneous reactive crystallization. Hydrometall. 2020, 195, 105386. [CrossRef] 11. Linneen, N.; Bhave, R.; Woerner, D. Purification of industrial grade lithium chloride for the recovery of high purity battery grade lithium carbonate. Sep. Purif. Technol. 2019, 214, 168–173. [CrossRef] 12. Zhu, C.; Dong, Y.; Yun, Z.; Hao, Y.; Wang, C.; Dong, N.; Li, W. Study of lithium exploitation from carbonate subtype and sulfate type salt-lakes of Tibet. Hydrometallurgy 2014, 149, 143–147. [CrossRef] 13. Martin, G.; Schneider, A.; Voigt, W.; Bertau, M. Lithium extraction from the mineral zinnwaldite: Part II: Lithium carbonate recovery by direct carbonation of sintered zinnwaldite concentrate. Miner. Eng. 2017, 110, 75–81. [CrossRef] 14. Xu, Z.; Zhang, H.; Wang, R. Systemic and Direct Production of Battery-Grade Lithium Carbonate from a Saline Lake. Ind. Eng. Chem. Res. 2014, 53, 16502–16507. [CrossRef] 15. Yi, W.T.; Yan, C.Y.; Ma, P.H. Removal of calcium and magnesium from Li2 HCO3 solutions for preparation of high-purity Li2 CO3 by ion-exchange resin. Desalination 2009, 249, 729–735. [CrossRef] 16. Xu, Z.G.; Wang, X.C.; Sun, S.Y. Performance of a Synthetic Resin for Lithium Adsorption in Waste Liquid of Extracting Aluminum from Fly-Ash. Chin. Chem. Eng. 2021. [CrossRef] 17. Shaojun, D.; Yuzhu, S.; Xingfu, S. Study on Preparation of Lithium Carbonate Via Reactive Crystallization from Old Salt Brine. Shandong Chem. Ind. 2018, 47, 5–8. 18. Weijun, L.B. Process analysis and mechanism discussion of enhanced COsequestration by mineral carbonation. Chem. Ind. Eng. Soc. China 2009, 60, 2332–2338. 19. Aghajanian, S.; Koiranen, T. Dynamic modeling and semibatch reactive crystallization of calcium carbonate through CO2 capture in highly alkaline water. CO2 Util. 2020, 38, 366–374. [CrossRef] 20. Yi, W.T.; Yan, C.Y.; Ma, P.H. Crystallization kinetics of Li2 CO3 from LiHCO3 solutions. Cryst. Growth 2010, 312, 2345–2350. [CrossRef]
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