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Industrial & Engineering Chemistry Research pubs.acs.org/IECR Article Figure 10. Li+ concentration over time in a 0.70 M LiCl solution containing (i) 1.4 M Na2SO4 (dashed lines with rhombus symbols, I = 4.90 M), (ii) 1.4 M Na2SO4 and 1.0 M KCl (I = 5.90 M, dot-dashed lines with triangle symbols), and (iii) without Na2SO4 (I = 4.20 M, dashed lines with square symbols, see Figure 5d). T = 50 °C. Stirring speed = 300 rpm, CO32−/Li+ ratio = 1, and Na2CO3 solution flow rate = 10 mL/min. 5d). Similar purity values are observed in high-ionic strength solutions with and without Br− ions (∼80%). 3.2. Lithium Precipitation with NaOH/CO2(g). The recovery of Li+ using a NaOH solution and CO2 gas insufflation represents a promising and environmentally friendly strategy for Li2CO3(s) production and CO2 capture. The influence of several operating parameters was investigated on lithium recovery adopting such a precipitation strategy, namely, (i) the influence of the OH−/Li+ ratio, (ii) the influence of temperature and solution ionic strength, and (iii) the influence of dissolved magnesium ions. 3.2.1. Influence of the OH−/Li+ Ratio. The influence of the OH−/Li+ ratio on Li2CO3(s) precipitation in a gas−liquid system was investigated within a OH−/Li+ mole ratio between 1 and 4. Experiments were conducted at 80 °C employing different 8.0 M NaOH volume solutions. The solution was steadily stirred at 300 rpm, and CO2 gas was fed at a flow rate of ∼4.5 L/h. Details of the reacting solutions are reported in Table S5 in the Supporting Information. In addition to the Li+ concentration variation along time, Figure 13 reports also the solution pH and indications on the Figure 13. Lithium concentration (dashed lines with square symbols) and pH (dot-dashed lines with cross-symbols) versus time for a OH−/ Li+ = 2. Li+ initial concentration after NaOH solution addition of ∼3900 ppm, T = 80 °C, and stirring speed = 300 rpm. CO2 flow rate ≈ 4.5 L/h. visual opacity threshold observed during the experiment, thus allowing a more phenomenological interpretation of the experiment. For the sake of brevity, such trends are reported only for the OH−/Li+ ratio of 2, although similar considerations hold for the other cases. Starting from time = 0, after the addition of the alkaline reactant and starting insufflating CO2, the solution pH increases slightly from 9.0 to 9.1 until the solution becomes turbid, indicating that Li2CO3 precipitation has started. Then, pH increases up to ∼9.4 to further sharply decrease to 8.5. At such a pH value, CO2(g) is stopped (40 min) to prevent a pH decrease, causing Li2CO3 “re-carbonation” (see the Supporting Information for further details). As for the pH, the Li+ concentration remains almost constant until the solution becomes turbid to suddenly drop to a value of ∼1300 ppm after 30 min, and then, it slightly increases again to a final concentration of ∼1450 ppm caused by very slight re- carbonation of Li2CO3. No further concentration variation is observed after CO2 interruption. − + The recovery and purity as a function of the OH /Li ratio are reported in Figure 14. https://doi.org/10.1021/acs.iecr.2c01397 Figure 11. Li+ concentration over time in a 0.70 M LiCl solution containing (i) 1.0 M NaBr (I = 1.70 M, dotted lines with rhombus symbols), (ii) 1.1 M KCl and 1.0 M NaBr (I = 2.80 M, dot-dashed lines with triangle symbols), and (iii) without NaBr (I = 4.20 M, dashed lines with square symbols, see Figure 5d). T = 50 °C, stirring speed = 300 rpm, CO32−/Li+ ratio = 1, and Na2CO3 solution flow rate = 10 mL/min. Li+ concentration close to that in high-ionic strength solution without dissolved Br− ions (I = 4.20 M) is observed. Figure 12 shows purity and recovery values for Li2CO3 solids precipitated from solutions containing Br− ions. A Li recovery of ∼47% is found in the presence of Br− ions, which increases up to 63% in higher-ionic strength solutions, almost as that in the case with no Br− ions (72%, see Figure Figure 12. Lithium recovery and purity for Li2CO3(s) precipitation experiments in the presence of Br ions. 13596 Ind. Eng. Chem. Res. 2022, 61, 13589−13602PDF Image | Recovery of Lithium Carbonate from Dilute Li Rich Brine
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