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3.2.1. NF Process The corresponding experimental results are shown in Figure 3 and Table 3. As shown in Figure 3a, the initial operation pressure of the nanofiltration was 2.0 MPa. The water flux decreases slowly from the initial 52 L·m−2·h−1 to 50.5 L·m−2·h−1 at first, and then rapidly declines from 50.5 L·m−2·h−1 to Membranes 2020,−210,−3171 7 of 14 31.6 L·m ·h . Inversely, the operation pressure increases at first and then rapidly reaches 8 MPa. There are three main reasons for this phenomenon: (1) the increase of the osmotic pressure in the retentate solution; (2) the precipitation of the salts on the surface of the NF membrane; and (3) the 3.2. NF and RO Processes compaction of the NF membrane. The concentration of the ions in the permeate flow and collected retentate during the NF process In order to precipitate lithium carbonate, the lithium-riched anolyte needs to be deeply purified are shown in Table 3 and Figure 3b, respectively. From Table 3, it can be seen that the conductivity and concentrated. In this paper, NF and RO were used for deep purifying of the divalent ions and increased slowly at the beginning of the initial stage (increased from 37.5 mS·cm−1 to 52.0 mS·cm−1). concentrating of the penetrating fluid, respectively. Both NF and RO were carried out only once and Subsequently, a significant increase followed after 90 min from the start of the NF, and the the corresponding results of the NF and RO processes are shown in below. conductivity reached 108.2 mS·cm−1. The temperature rose slowly throughout the experiments (from 24.7 °C to 27.5 °C), and the rise in water temperature comes from two aspects: (1) the mechanical 3.2.1. NF Process friction of the high pressure pump produce a great deal of heat; and (2) the friction of the fluid and the pipe, which also generates heat. The flow rate of the entire NF process was kept at 16 L·min−1. The corresponding experimental results are shown in Figure 3 and Table 3. As shown in Figure 3a, There was no significant change in the concentration of monovalent ions such as Li+, Na+, and K+, the initial operation pressure of the nanofiltration was 2.0 MPa. The water flux decreases slowly from while divalent ions such as Mg2+, Ca2+, and SO42− are abundantly enriched in the retentate solution. the initial 52 L·m−2·h−1 to 50.5 L·m−2·h−1 at first, and then rapidly declines from 50.5 L·m−2·h−1 to Moreover, the concentration of Mg2+, Ca2+, and SO42− at the end of the NF process reached 18.23 g·L−1, 31.6 L·m−2·h−1. Inversely, the operation pressure increases at first and then rapidly reaches 8 MPa. 0.02 g·L−1, and 2.41 g·L−1, respectively. It can be found that Mg2+, Ca2+, and SO42− were concentrated 9.3 There are three main reasons for this phenomenon: (1) the increase of the osmotic pressure in the times, 5 times, and 9.1 times, respectively. The concentrated times of Ca2+ were lower than those of retentate2+ solution2;−(2) the precipitation of the salts on the surface of the−NF membrane; and (3) the Mg and SO4 . Notably, the main anion in the collected retentate is Cl , which was rejected to compaction of the NF membrane. maintain the electrical neutrality of the collected retentate. Figure 3. The NF process for purification. (a) The relationship of the operation pressure and the flux of the membrane; (b) concentration of Li+, Na+, K+, Mg2+, Ca2+, and SO42− in the permeate flow; (c) the rejection rate of Mg2+ and SO42−; (d) the recovery of lithium and the separation factor of lithium and magnesium (SFLi-Mg). Table 3. The main analytical results in the collected retentate during the nanofiltration (NF) process. Time min 0 30 60 90 105 Conductivity T Flow ms·cm−1 ◦ C L·min−1 Li+ Na+ 37.5 24.7 16 2.10 1.91 40.9 25.3 16 2.26 1.82 44.9 26.2 16 2.32 1.91 52.0 27.0 16 2.28 1.69 108.2 27.6 16 2.31 1.96 Concentration of Ions/g·L−1 K+ Mg2+ 0.04 1.95 0.038 3.64 0.037 5.34 0.036 9.78 0.041 18.23 Ca2+ Cl− 0.0053 24.5 0.35 SO42− 0.004 19.1 0.26 0.0085 30.2 0.56 0.018 42.1 1.21 0.02 66.8 2.37 The concentration of the ions in the permeate flow and collected retentate during the NF process are shown in Table 3 and Figure 3b, respectively. From Table 3, it can be seen that the conductivityPDF Image | Membrane Process for Preparing Lithium Carbonate
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