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Industrial & Engineering Chemistry Research pubs.acs.org/IECR Article Figure 2. (a) Schematic representation of the employed experimental setup for lithium precipitation with sodium carbonate: (1) six-position magnetic stirrer, (2) double-walled beaker, (3) heating water from a thermostatic bath, (4) peristaltic pump, (5) 250 mL volume beakers, (6) oven, (7) PT100 temperature probe. Pictures of the experimental setup; (b) six-position magnetic stirrer with precipitated lithium carbonate placed in an oven. (c) Whole experimental set up. influence the Li2CO3(s) particle size. The use of a falling film column was also investigated, some years later, by Sun et al.24 for the same Li2CO3(s) precipitation process in the LiOH− CO2 system. Tian et al.25 studied the influence of ammonium hydroxide (NH3·H2O) in the gas−liquid reactive crystalliza- tion of Li2CO3(s). The ammonium ions were believed to greatly influence the Li2CO3(s) precipitation process by inhibiting the re-carbonation of Li2CO3(s). Zhou et al.26 used a coupled reaction and solvent extraction process to produce Li2CO3(s) from the LiCl and CO2(g) system. HCl was removed, to increase the reaction yield, by solvent extraction using tri-n-octyl amine and iso-octanol as solvent. Han et al.19 presented a comparison between homogenous Li2CO3 precipitation using only soda ash and heterogeneous Li2CO3 precipitation employing NaOH and the addition of CO2(g) from Li2SO4 solutions mimicking a waste solution of lithium-containing electrical and electronic equipment. Results showed that both methods can be feasible to recover lithium as lithium carbonate salt from Li2SO4 solutions. On the basis of the above literature review, it is clear how the Li2CO3 precipitation process has been extensively studied in the past. However, Li+ precipitation has been mostly studied in highly Li-concentrated solutions, with Li+ concentrations higher than 10,000 ppm,11,19,23,27 with less studies addressing low Li-containing ones, with concentrations lower than 5000 ppm (as in ref 28). Nevertheless, lithium extraction from seawater, brines, and bitterns requires a preliminary concen- tration step to increase lithium concentrations from tens to thousands of ppm, highlighting the importance of character- izing the precipitation phenomena at low concentration than in conventional processes. The present paper aims at reporting an extensive experimental campaign to prove the feasibility and provide the most favorable strategies for the recovery of Li+ from low- concentration solutions (Li+ concentration ∼ 4000 ppm). Here, attention is on Li+ recovery and purity determined in several precipitation cases. Specifically, Li2CO3(s) precipitation was studied following two precipitation routes: (i) using Na2CO3 solution and NaOH solution and CO2(g) insufflation. Several parameters affecting both precipitation routes were investigated, such as Li+/precipitant ratios, solution temper- ature, and the presence of dissolved monovalent and divalent ions, which can be present in the eluate of Li-MFCDI from the feed bittern (e.g., Na+, K+, Cl−, SO42−, etc.) and could be further concentrated before crystallization. A purification step using ethanol was also studied to enhance Li2CO3 solid purity. In regard to the NaOH solution and CO2(g) insufflation route, to the best of the author knowledge’s, there are no other studies reporting Li+ purity and recovery in Li solutions containing dissolved monovalent and divalent ions mimicking real Li+ solutions. Results provide straightforward and useful information for the design of Li2CO3 crystallizers for the recovery of lithium from low-Li-concentration solutions. 2. MATERIALS AND METHODS All precipitation experiments were performed on a laboratory- scale setup, preparing synthetic solutions of LiCl, plus other salts (as simulated feed brine) and Na2CO3 or NaOH as precipitation inducing reactants. Details on materials, exper- imental setups, and procedures are reported in the following sections, while for the sake of brevity, a complete description of the two investigated precipitation routes and a literature overview of previous studies focused on Li2CO3 precipitation fundamentals are reported in the Supporting Information. 2.1. Materials. Table S1 in the Supporting Information lists all chemicals used in the Li+ precipitation experiments. The reagents were of analytical grade and were employed without further purification. Deionized water was used for all experiments. Synthetic solutions were prepared by dissolving the desired salts weighted using a precision balance (Sartorius BCE 653) in a beaker filled with deionized water to a defined total mass of salts and water of ∼110 g. The precise mass for https://doi.org/10.1021/acs.iecr.2c01397 13591 Ind. Eng. Chem. Res. 2022, 61, 13589−13602PDF Image | Recovery of Lithium Carbonate from Dilute Li Rich Brine
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