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Membranes 2020, 10, 371 3 of 14 2.2. Experimental Illustration 2.2.1. Methods LiFePO4/FePO4 electrodes’ preparation: LiFePO4 electrode was prepared as follows: (1) weighing LiFePO4, polyvinylidene fluoride (PVDF), and acetylene black (C) in a mass ratio of 8:1:1; (2) dissolving PVDF into N-methylpyrrolidone (NMP) and then adding C and LiFePO4 in order; (3) coating the above-mixed slurry on a carbon fiber sheet; and (4) drying the prepared carbon fiber sheet in a vacuum oven at 95 ◦C for 12 h. The FePO4 electrode was obtained by deintercalating lithium from the LiFePO4 electrode. Concretely, an electrolytic cell is divided into an anode chamber and cathode chamber by anion membrane, LiFePO4 electrode (anode) and nickel foam (cathode) were placed into the anode and cathode chamber, respectively. Both of the chambers were filled with 5 g·L−1 NaCl solution and the pH value of the catholyte was controlled to 2–3 using HCl. The voltage used in electrolysis is 1.0 V, and the electrolysis ends until the current density is less than 0.05 mA·cm−2. EID method for lithium extraction: The device for the EID method is shown in our previous work [20]. The device of the EID system was divided into two chambers by the anion membrane, where LiFePO4 and FePO4 is used as anode and cathode, respectively. The anode and cathode chambers are filled with supporting electrolyte and brine, respectively. The entire working process is shown below: (1) lithium deintercalated from LiFePO4 to the supporting electrolyte (LiFePO4 – e = Li+ + FePO4); (2) lithium existed in the brine intercalated into FePO4 (Li+ + FePO4 + e = LiFePO4); and (3) the Cl− in the brine diffused into the anode chamber through the anionic membrane to maintain the electroneutrality of the anolyte and brine, and LiCl was obtain in the anolyte. The brine used for the lithium extraction was from West Taijnar Salt Lake (Golmud, China) with the Mg/Li ratio of 58.8 (Table 1), and the lithium extraction process was carried out via instrument LANHE-CT2001A (Wuhan, China). The effective size of the electrodes was 17 × 20 cm2, and the electrodes of LiFePO4 and FePO4 worked as anode and cathode, respectively. The electrode coating density was about 85 mg (LiFePO4)·cm−2. The electrolytic cell was comprised of two chambers, which were separated by an anion exchange membrane (MA-3475, Beijing Anke Membrane Separation Technology Engineering Co. LTD, Beijing, China agent). The anode chamber was filled with 1.5 L of 5 g·L−1 NaCl as supporting electrolyte, and the cathode chamber was filled with 1.5 L brine. The entire electrolysis was performed with a constant current of 0.6 A until the voltage reached 0.35 V, and then worked at a constant voltage until the current dropped to 0.1 A to end the electrolysis process. Table 1. The components of the West Taijnar Salt Lake brine (g·L−1). Element Li+ Na+ K+ Mg2+ Ca2+ SO42− Cl− West Taijnar 2.05 0.81 0.48 120.56 0.04 31.01 360.9 NF for purification: The obtained anolyte was purified by NF, the volume of the feed used in the nanofiltration was 200 L, and the composition of the feed used was configured according to the composition of the anolyte obtained by the EID system. The NF process was carried out at a constant pump power of 2 KW until the operation pressure reached 8 MPa. The total volume of the collected permeate solution was 180 L. RO for concentration: The collected permeate solution after the NF treatment was concentrated by RO process, and only 175 L feed liquor was used in the process. The whole RO process was performed at the room temperature and ended until the volume of permeate reached 105 L. The RO process was also carried out at a constant pump power of 2 KW. Evaporation and concentration: The evaporation process was carried out by an electric furnace, and the initial volume of the solution used for the evaporation was 5 L. Precipitation of Li2CO3: The lithium-containing solution after evaporation process was precipitated by Na2CO3 (280 g·L−1) at 95 ◦C. The addition of sodium carbonate is 1.05 times the dosage of theoreticalPDF Image | Membrane Process for Preparing Lithium Carbonate
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