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Materials 2019, 12, 1968 5 of 13 2.2.2. Slurry Concentration of LiAl-LDHs-1 LiAl-LDHs-1 were dispersed in water at slurry concentrations of 10, 20, 30, or 50 g/L at 85 ◦C for 90 min. 2.2.3. Lithium Recovery Temperature LiAl-LDHs-1 were dispersed in water at a slurry concentration of 10 g/L. The temperature of the thermal reaction was 65, 75, 85, or 95 ◦C. The reaction time was 90 min. 2.2.4. Lithium Recovery Time LiAl-LDHs-1 were dispersed in water at a slurry concentration of 10 g/L at 85 ◦C. The reaction time was set at 30, 60, 90, or 120 min. 2.3. Analysis The X-ray diffraction patterns were obtained from XRD-6000 diffractometer (Shimadzu, Kyoto, Japan) in which the radiation was Cu Kα radiation at a sweep speed of 10◦/min from 3◦ to 70◦. The Cl and C elements mass percentage were determined by ion chromatography (ICS-5000, ThermoFisher Scientific, Waltham, MA, USA) and elemental analysis (vario EL CUBE, elementar Analysensysteme GmbH, Langenselbold, Germany). The solid sample was dispersed with ethanol and dripped onto a carbon-coated Cu grid, and the morphology of the sample was observed using transmission electron microscopy (HT7700, Hitachi, Tokyo, Japan). Solid-state nuclear magnetic resonance examined the coordination information of 27Al and 7Li using NMR equipment (AV300, Bruker BioSpin GmbH, Rheinstetten, Germany). The composition and chemical structure of LiAl-LDHs and solid products after lithium recovery were characterized by X-ray photoelectron spectroscopy (ESCALAB 250, ThermoFisher Scientific, Waltham, MA, USA). The concentration of the metal ion to be measured in solid and liquid phase products was diluted to 0–100 ppm to detect lithium ions and aluminum ions by inductively coupled plasma mass spectrometry (ICPS-7500 from Shimazduo, Kyoto, Japan). The formulas for Li+ concentration in the filtrate, lithium recovery percentage, and Al3+ dissolution percentage are shown in the Supplementary Materials Calculation Section. 3. Results and Discussion LiAl-LDHs with varied initial Li+ concentrations were prepared from salt lake brine. The chemical compositions of the prepared LiAl-LDHs are listed in Table 2. The Li/Al molar ratio of LiAl-LDHs-1, LiAl-LDHs-2, and LiAl-LDHs-3 were 1:2.00, 1:2.02, and 1:2.14, respectively, which are consistent with stoichiometry. The mass percentage of Cl element was 14.05%, 14.02%, and 13.89%, and the Li/Cl molar ratio was 1.00. The Cl/C molar ratio of LiAl-LDHs-1, LiAl-LDHs-2, and LiAl-LDHs-3 were 9.90, 9.88, and 9.80, respectively (Table 2), which indicated that the amount of CO32- in LiAl-LDHs was negligible. The XRD pattern (Figure 1) demonstrated that the diffraction line was consistent with planes (002), (101), (004), (112), (106), (008), (303), and (1010) of [LiAl2(OH)6]Cl·xH2O (JCPDS Card No. 51-0357) [25,26]. The chlorine-ion-intercalated LiAl-layered double hydroxides were prepared via a mild solution chemistry process from salt lake brine. The higher the lithium ion concentration, the sharper the diffraction peak, which indicated that the crystallinity of LiAl-LDHs-1, LiAl-LDHs-2, and LiAl-LDHs-3 decreased in turn. As shown in Figure 2, the crystal growth of LiAl-LDHs was complete and displayed a hexagonal sheet morphology, which is characteristic of LDHs, and the crystallization is consistent with the XRD pattern [27,28]. The 27Al NMR spectra (Figure S1) of LiAl-LDHs-1 revealed a chemical shift of 27Al as 6.39 ppm; that is, the Al environment was six-coordinated Al [29]. This result was consistent with researchers’ understanding of LiAl-LDHs [26]. The XPS O 1s spectra ofPDF Image | Lithium Recovery Pre-Synthesized Chlorine-Ion-Intercalated
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