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Membranes 2020, 10, 371 10 of 14 Membranes 2020, 10, x FOR PEER REVIEW 10 of 14 Figure 4. The main results in the RO process. (a) The relationship of the operation pressure and Figure 4. The main results in the RO process. (a) The relationship of the operation pressure and the the flux of the membrane; (b) concentration of Li+, Na+, K+, and Mg2+ in the collected retentate; flux of the membrane; (b) concentration of Li+, Na+, K+, and Mg2+ in the collected retentate; (c) (c) concentration of Li+, Na+, K+, and Mg2+ in the permeate flow. concentration of Li+, Na+, K+, and Mg2+ in the permeate flow. The final composition of the permeate flow and the collected retentate produced by RO is shown The final composition of the permeate flow and the collected retentate produced by RO is shown in Table 6. As shown in Table 6, the concentration of ions in the permeate flow is very low, the loss of in Table 6. As shown in Table 6, the concentration of ions in the permeate flow is very low, the loss the lithium in the RO permeate flow almost can be ignored, and the recovery of lithium can reach 99.4%. of the lithium in the RO permeate flow almost can be ignored, and the recovery of lithium can reach Moreover, the permeate flow with such a low salinity content can be used to prepare the supporting 99.4%. Moreover, the permeate flow with such a low salinity content can be used to prepare the electrolyte for the EID system. supporting electrolyte for the EID system. Table 6. The final compositions of the permeate flow and collected retentate. Table 6. The final compositions of the permeate flow and collected retentate. Li+ Na+ Li+ Na+ K+ K+ Mg2+ Ca2+ Mg2+ Ca2+ 0.002 / 0.002 / SO 2− SO42−4 / The concentrations of L+i+ and M2+g2+ after RO are 5.4 −g1 ·L−1 and 0.525−1 g·L−1, respectively. The concentrations of Li and Mg after RO are 5.4 g·L and 0.525 g·L , respectively. This This solution cannot be used directly for the precipitation of Li CO , and generally requires evaporation solution cannot be used directly for the precipitation of Li2C2O3, 3and generally requires evaporation Elements Lithium Recovery % Elements Lithium Recovery % Permeate flow 0.021 0.011 −4 4 × 10−4 / / Permeate flow 0.021 0.011 4 × 10 −4 0.525 6.3 × 10−4 / Collected retentate 5.4 4.4 0.08 0.525 6.3 × 10 0.003 99.4 Collected retentate 5.4 4.4 0.08 0.003 99.4 3.3. Precipitation of Li CO 3.3. Precipitation of Li22CO33 and impurity removal. Subsequently, we use an electric furnace to evaporate 5 L of solution to and impurity removal. Subsequently, we use an electric furnace to evaporate 5 L of solution to 1.2 L, 1.2 L, and add NaOH to adjust the pH of the solution to 12.5 for further removal of magnesium2+ and add NaOH to adjust the pH of the solution to 12.5 for further removal of magnesium (Mg (Mg2+ precipitates in the form of Mg(OH) when the solution is alkaline). The composition of the precipitates in the form of Mg(OH)2 when t2he solution is alkaline). The composition of the solution solution after magnesium removal is shown in Table 7. after magnesium removal is shown in Table 7. −1 Table 7. The composition of the solution after magnesium removal (g·L −1 ). Table7.Thecompositionofthesolutionaftermagnesiumremoval(g·L ). Elements Li+ Na+ K+ Elements Li Na K ConcenCtornactieonntration2211.6.6 2233..9 00.3.34 Mg 2+ Mg Ca 2+ Ca Lithium Recovery % + + + 2+ 2+ SO 2−2− SO4 4 00.0.01188 Lithium Recovery % 0.002 −-4 2.29.9××10 96.1 96.1 As shown in Table 7, the concentration of Li+ is enriched to 21.6 g·L−1; the mass ratio of Na/Li is As shown in Table 7, the concentration of Li+ is enriched to 21.6 g·L−1; the mass ratio of Na/Li is slightly greater than 1; and other ions such as K+, Mg2+, Ca2+, and SO42− are very low. The recovery of slightly greater than 1; and other ions such as K+, Mg2+, Ca2+, and SO42− are very low. The recovery lithium in this process can reach 96.1%; such a low lithium loss is attributed to the effective removal of lithium in this process can reach 96.1%; such a low lithium loss is attributed to the effective removal of magnesium by the NF, which greatly reduces the generation of Mg(OH)2 and improves the of magnesium by the NF, which greatly reduces the generation of Mg(OH)2 and improves the recovery recovery rate of lithium. In the actual production process, the water generated by evaporation can rate of lithium. In the actual production process, the water generated by evaporation can also be also be returned to the EID system to prepare the supporting electrolyte. returned to the EID system to prepare the supporting electrolyte. The solution with 21.6 g·L−1 lithium was used for the precipitation of Li2CO3 with 280 g·L−1 The solution with 21.6 g·L−1 lithium was used for the precipitation of Li2CO3 with 280 g·L−1 Na2CO3. Moreover, the concentration of the mother liquor is shown in Table 8. From Table 8, it can Na2CO3. Moreover, the concentration of the mother liquor is shown in Table 8. From Table 8, it can be be seen that the main ions in the mother liquor are Na+ and Li+. Noteworthily, only 86.7% lithium was seen that the main ions in the mother liquor are Na+ and Li+. Noteworthily, only 86.7% lithium was precipitated by Na2CO3, and the concentration of lithium in the mother liquor is still 1.8 g·L−1. In the precipitated by Na2CO3, and the concentration of lithium in the mother liquor is still 1.8 g·L−1. In the same way, the mother liquor contains a small amount of excess carbonate, which can be neutralized same way, the mother liquor contains a small amount of excess carbonate, which can be neutralized by by part of the brine with high Mg2+ ions, and then the mother liquor is returned to the EID system to recover the residual lithium.PDF Image | Membrane Process for Preparing Lithium Carbonate
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