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Industrial & Engineering Chemistry Research pubs.acs.org/IECR Article Figure 3. (a) Schematic representation of the experimental setup employed for lithium carbonate precipitation with sodium hydroxide and carbon dioxide insufflation: (1) carbon dioxide bottle, (2) needle valve, (3) bubble counter with a regulator, (4) PE hose for CO2 insufflation Ø 0.5 mm, (5) PT100 thermocouple probe (6) magnetic stirrer with a heating plate, (7) 250 mL beaker, (8) pH electrode with a measuring device. (b) Picture of the experimental setup during Li2CO3 precipitation. each experiment is reported in the relevant tables in the Results and Discussion section. The total volume was determined by measuring the solution density with a DMA 35 density meter (Anton Paar) and knowing the total mass of the solution. LiCl solutions of ∼5000 ppm (0.70 M) were prepared aiming at obtaining an initial Li+ concentration of ∼4000 ppm (0.59 M) after reactant solution addition (which generates a further dilution of the initial feed solution at time to, at which reaction has not started yet due to the low precipitation kinetics). Exact concentrations for each experiment are reported in the relevant tables in the Results and Discussion section. 2.2. Experimental Setup and Procedure for Li+ Precipitation with Na2CO3. The employed experimental setup for Li2CO3 precipitation tests using Na2CO3 solutions is presented in Figure 2. The synthetic brines were stirred steadily in a thermostatic room on a six-position magnetic stirrer and covered with Parafilm to avoid evaporation losses. The temperature of the samples was indirectly checked by measuring the temperature of a blank sample consisting of a beaker filled with a comparable amount of water, via a Pt100 temperature probe. All solutions were stirred at a speed of 300 rpm. The temperature of the Na2CO3 solution, to be injected into the abovementioned samples, was controlled using a double-walled beaker connected to a thermostat and set to the same temperature as that of the thermostatic room where the precipitation took place. After reaching the desired constant temperature, the desired volume of a 2.0 M Na2CO3 solution was added to the Li+-containing solution with a peristaltic pump (SIMDOS 02) at a flow rate of 10 mL/min; the same flow rate and solution concentration were used in all the experiments, unless stated otherwise. In all experiments, the reaction time is considered to start after the complete addition of the Na2CO3 solution volume. + 2.3. Experimental Setup and Procedure for Li Precipitation with NaOH and CO2(g). The experimental setup employed for Li2CO3(s) precipitation with NaOH and CO2(g) insufflation is shown in Figure 3. In this case, an 8.0 M NaOH solution (32 % wt) was employed. The NaOH/LiCl solution was placed in a 250 mL beaker heated and stirred using a RET control-visc white stirrer from IKA, which offers a heating plate whose temperature is controlled based on a feedback signal acquired by a submersed Pt100 temperature probe. When the solution reached the desired temperature, CO2(g) was supplied through a polyethylene (PE) hose with an inner diameter of 0.5 mm. The hose was placed close to the stirrer to better disperse the gas bubbles and prevent any clogging. To minimize water losses due to evaporation, the beaker was covered with Parafilm. The CO2(g) feed rate was adjusted by using a needle valve and a downstream bubble counter. The pH was continuously monitored in the precipitation beaker via a temperature-compensated SenTix precision electrode from WTW. 2.4. Sampling and Analytical Procedures. For the quantitative determination of cation concentration in the reacting solution, from which Li+ recovery can be calculated, samples were withdrawn with pre-heated syringes (kept at the reaction temperature, to prevent any Li2CO3(s) dissolution). After sampling, the solution was filtered with a Berrytec nylon syringe filter (0.22 μm) and directly diluted 1:100 to interrupt the precipitation kinetics. The solutions were further diluted, and their composition was measured by employing a multiparameter optical emission spectrometer (ICP−OES, Varian 720-ES type). Multiple determinations of individual measurement points were carried out with a standard deviation of 3%. ICP−OES measurement accuracy was also verified by comparing ICP− OES concentration, measured at the beginning of the experiment, with the one expected from the mass of lithium dissolved in the feed. A deviation lower or equal to 4% was determined in all cases. For the sake of graphical clarity in all plots, the relevant error bars are not reported as they would coincide with the size of the symbols. To determine Li2CO3 solid purity, the precipitated solid samples were separated by vacuum filtration with a Büchner funnel using a cellulose acetate filter having a pore size of 0.45 μm. After filtration, the crystals were dried in a moisture analyzer (DLB-160-3A by Kern) at 105 °C for 12 h. Part of the dried precipitate was re-dissolved in a 1% HNO3 solution and further diluted with deionized water. Subsequently, the concentration of dissolved lithium was determined by ICP− OES (see above). In selected experiments, the precipitate was washed in order to increase its purity. For this purpose, ∼0.1 g of Li2CO3 was weighted and then suspended in 50 mL of ethanol (w = 70%) solution at room temperature for 1 h. After this step, the precipitate was filtered again, and the purity in Li+ was determined by ICP−OES. 2.5. Precipitation Performance Parameters. In all the performed experiments, the recovery of lithium was assessed. It was calculated as the difference between the initial and final https://doi.org/10.1021/acs.iecr.2c01397 13592 Ind. Eng. Chem. Res. 2022, 61, 13589−13602PDF Image | Recovery of Lithium Carbonate from Dilute Li Rich Brine
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