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Materials 2019, 12, 1968 7 of 13 Materials 2019, 12, x FOR PEER REVIEW 7 of 13 such they cannot be used as evidence for identifying substances because they are weaker diffraction signals. In order to further discuss the relationship between lithium recovery and crystallinity2,7 we crystallinity, we studied the changes in Li+ concentration in the filtrate, the chemical shift of Al, studied the changes in Li+ concentration in the filtrate, the chemical shift of 27Al, and binding energy. and binding energy. Figure 3. XRD patterns of solid products after lithium recovery from LiAl-LDHs at varied initial Li+ Figure 3. XRD patterns of solid products after lithium recovery from LiAl-LDHs at varied initial Li+ concentrations (a) 6.75 g/L, (b) 3.375 g/L, (c) 1.6875 g/L ( Al(OH)3). concentrations (a) 6.75 g/L, (b) 3.375 g/L, (c) 1.6875 g/L (▲ Al(OH)3). The concentration of Li+ in the filtrate decreased with the decreasing of crystallinity because The concentration of Li+ in the filtrate decreased with the decreasing of crystallinity because the the amount of Li+ extracted decreased from LiAl-LDHs (Table 3). Because of the low crystallinity, amount of Li+ extracted decreased from LiAl-LDHs (Table 3). Because of the low crystallinity, the the distortion of AlO6 octahedrons occurred. The Al-O chemical bonds were broken under the mild distortion of AlO6 octahedrons occurred. The Al-O chemical bonds were broken under the mild chemistry process, allowing a small amount of Al3+ to be dissolved in the solution. chemistry process, allowing a small amount of Al3+ to be dissolved in the solution. Table 3. Analyses on the solution after lithium recovery from LiAl-LDHs at varied initial Ta+ble 3. Analyses on the solution after lithium recovery from LiAl-LDHs at varied initial Li+ Li concentrations. concentrations. Sample Sample LiAl-LDHs-1 Lithium Recovery Li+ Concentration Li+ Concentration Al3+ Dissolution Al3+ Dissolution LiAl-LDHs-1 - 66.6 127.4 - LiAl-LDHs-2 LiLAilA-Ll-DLHDsH-3s-2 LiAl-LDHs-3 86.2 141.6 - Lithium Recovery in Filtrate (mg/L) in Filtrate (mg/L) Percentage (%) Percentage (%) Percentage (%) Percentage (%) 86.2 141.6 656.26 112077.4.4 - 0.32 56.2 107.4 0.32 The weight of LiAl-LDHs is 1 g. The volume of the solution after the experiment is 167 mL, 143 The weight of LiAl-LDHs is 1 g. The volume of the solution after the experiment is 167 mL, mL, and 142 mL for LiAl-LDHs-1, LiAl-LDHs-2, and LiAl-LDHs-3, respectively. 143 mL, and 142 mL for LiAl-LDHs-1, LiAl-LDHs-2, and LiAl-LDHs-3, respectively. +- The dissolution of Li + with Cl - from LiAl-LDHs into aqueous solution changes the Al-O The dissolution of Li with Cl from LiAl-LDHs into aqueous solution changes the Al-O coordination environment of solid products after lithium recovery. The recovery rate of lithium from coordination environment of solid products after lithium recovery. The recovery rate of lithium LiAl-LDHs-1 reached 86.2% to deform the Al-O octahedron [32], and the chemical shift of 27Al w27as from LiAl-LDHs-1 reached 86.2% to deform the Al-O octahedron [32], and the chemical shift of Al shifted from 6.39 ppm (27Al27chemical shift of LiAl-LDHs-1, Figure S1) to the low-field by 0.32 ppm was shifted from 6.39 ppm ( Al chemical shift of LiAl-LDHs-1, Figure S1) to the low-field by 0.32 ppm (Figure 4). Moreover, the chemical shifts of LiAl-LDHs-2 and LiAl-LDHs-3 were shifted to the (Figure 4). Moreover, the chemical shifts of LiAl-LDHs-2 and LiAl-LDHs-3 were shifted to the low-field low-field by 0.24 and 0.09 ppm, respectively. The chem2i7cal shift of 27Al was shifted towards the by 0.24 and 0.09 ppm, respectively. The chemical shift of Al was shifted towards the low-field with low-field with increasing crystallinity of LiAl-LDHs. Larger lithium recovery percentage lead to a increasing crystallinity of LiAl-LDHs. Larger lithium recovery percentage lead to a greater impact on greater impact on aluminum coordination. aluminum coordination.PDF Image | Lithium Recovery Pre-Synthesized Chlorine-Ion-Intercalated
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