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Industrial & Engineering Chemistry Research pubs.acs.org/IECR Article increased by using high-ionic strength solutions, reaching the highest measured recovery value of 80% when using NaOH and CO2 insufflation at 80 °C. On the other hand, purity values range from 65 to 90% in high-ionic strength solution or in the presence of Mg ions. Conversely, solids produced from pure LiCl solutions exhibit purities higher than 94%. The ethanol washing step allows the production of 100% pure solids, causing, however, a Li+ reduction of equivalent recovery that ranges from 45 to 63%. Results also highlight that the Li2CO3(s) precipitation using NaOH solutions and CO2 insufflation can be pursued as a promising alternative for the simultaneously recovery of Li+ and CO2 capture since results are similar to those obtained using the classical Na2CO3 precipitant, especially due to the option of enhancing the purity by a simple filtration step without losing the product in the presence of divalent ions. Li2CO3 reaction times can also be compared between results of the two precipitation approaches, see Figures 5 and 15. Specifically, precipitation times were selected when Li+ concentrations did not vary more than 10% in two consecutive measurements. Table 2 reports a comparison between the precipitation times at 50 and 80 °C in LiCl solutions with and without salt addition. Table 2. Comparison of the Reaction Times during Li2CO3 Precipitation Tests that contain a Li+ concentration of 879 mg/L. The brine was first treated with Na2CO3 to reduce Ca2+ and Mg2+. Afterward, a conventional electrodialysis process was employed to increase the Li+ concentration up to 3485 mg/L. The concentrated solution had also 7319, 5.3, and 37 mg/L concentrations of Na+, Ca2+ and Mg2+. After Li2CO3 precipitation, a secondary crystallization step was adopted to increase powder purity from 90.33 to 95.30%. Unfortunately, the authors did not provide information regarding Li+ recovery. Um and Hirato35 studied the recovery of lithium from seawater adopting an adsorption Li+ selective step with the manganese oxide adsorbent and a further precipitation step. The obtained brine was treated using NaOH to reduce Ca2+ and Mg2+. Na2CO3 solution was added into the Li solution that was concentrated by evaporation at 100 °C, decreasing the solution volume to 67, 53, and 40%. The Li2CO3 yield varied from 51 to 77%; however, the purity decreased from 99.4 to 98.7%. Xu et al.36 developed a two-step process to produce battery-grade lithium carbonate from the Damxungcuo saline lake brine (Tibet). The brine contained 360 mg/L Li+, 54,000 mg/L, 7,300 mg/L, and 810 mg/L Na+, K+, and Mg2+, respectively. Li2CO3 solids were first produced by evaporation of saline lake solutions and then added to the Li brine. Lime milk and H2O2 were employed to remove insoluble compounds, NaOH was added to deplete Fe species concentration, and oxalic acid was added to remove Mg(OH)2 and Na2CO3 to treat Ca. After purification, industrial-grade Li2CO3 was obtained that was further treated using CO2 and EDTA-Li (lithium 2- carboxyhydrazine-1,1,2-tricarboxylate) at 85 °C to increase its purity up to 99.6% with a recovery of about 84%. Zhao et al.27 studied the recovery of lithium carbonate from synthetic lithium chloride solutions using ultrasounds. Lithium sulfate solutions with a Li concentration between 5000 and 25,000 mg/L were obtained from the leachate of the cathode scrap of lithium-ion batteries. The precipitation process was conducted at 70 °C. Na2CO3 was added at one time, immediately applying ultrasounds. Recovery and purity were compared with those of classical stirred precipitation systems without the use of ultrasounds. Recovery increased adopting ultrasound varying from 45 to 60 and from 70 to 80% for an initial Li+ concentration of 5000 and 10,000 mg/L, respectively. Purity also increased using ultrasounds, showing values higher than 98% at such concentrations. Quintero et al.37 developed a process for the direct production of magnesium-doped Li2CO3 solids by direct co-precipitation of Mg(OH)2 treating industrial Li-enriched brines. An industrial refined brine from the Albemarle industrial plant (North of Chile) was used with a concentration of 0.030, 1.14, 0.04, 0.02, and 3.22 % wt for Ca2+, Mg2+, Na+, K+, and Li+, respectively. Ca2+ was removed by using oxalate and NaOH solutions. Furthermore, NaOH was added to precipitate the remaining magnesium. Na2CO3 solution was used at a 1:2 Li+ ratio to co-precipitate Li2CO3. The Li2CO3 precipitation process occurred with a Li+ initial concentration of 30,000 ppm performed at 80 °C. The Li2CO3/Mg(OH)2 solid recovery was 88%. Table 3 reports a comparison between Li2CO3 precipitation approaches presented in the literature and the best scenarios addressed in the present work. Results indicate how the NaOH and CO2 (g) precipitation route conducted at 80 °C in a high-ionic strength Li solution leads to final Li recovery and purity values not too far from those of the other presented approaches in the literature. Specifically, a recovery of 80% is slightly lower than the other https://doi.org/10.1021/acs.iecr.2c01397 temperature Na2CO3 NaOH and CO2(g) [°C] solution [min] [min] 50 pure LiCl high ionic strength 80 pure LiCl high ionic strength 300 120 60 60 60 60 60 50 Li2CO3 precipitation is faster at 80 °C, showing similar reaction times of about 50−60 min for both precipitation approaches. Similar reaction times are also observed in high- ionic strength solutions. At 50 °C, the precipitation is faster in gas−liquid systems (120 min against 300 min for Na2CO3), while it is more than two times faster in high-ionic strength solutions. 3.4. Process Performance Comparison with the State of Art. For the sake of comparison with the state of art, an overview of recent literature studies is reported below for the Li2CO3 precipitation from Li brines, followed by a comparative table with the present work’s best identified scenario. An et al.33 presented a two-stage Li extraction process from Uyuni Salar brine (Bolivia) containing 700−900 mg/L Li+ and 15,000−18,000 mg/L Mg2+, among the other ions. First Mg2+, Ca2+, and sulfates were removed by precipitation using lime and sodium oxalate. Then, the purified brine was concentrated 30 folds by evaporation, reaching a final Li+ concentration of 20,000 mg/L. The concentrated brine also contained 56,000, 52,000, <0.05, 350, and 20,000 mg/L concentrations of Na+, K+, Ca2+, Mg2+, and SO42−, respectively. Li2CO3 precipitation was performed at 80−90 °C by the addition of Na2CO3. Li2CO3 solid purity was higher than 99.55%, after employing hot-water washing, while the recovery was estimated to be higher than 90%. Jiang et al.34 investigated the production of Li2CO3 from lithium brines adopting a laboratory-scale electrodialysis system. A synthetic brine was prepared to mimic the ion concentration in Zabuye lake brines (China) 13599 Ind. Eng. Chem. Res. 2022, 61, 13589−13602PDF Image | Recovery of Lithium Carbonate from Dilute Li Rich Brine
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