Lithium Recovery Pre-Synthesized Chlorine-Ion-Intercalated

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Lithium Recovery Pre-Synthesized Chlorine-Ion-Intercalated ( lithium-recovery-pre-synthesized-chlorine-ion-intercalated )

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Matteriialls2019,,12,,x19F6O8R PEER REVIEW 10off13 dissolved from the solid phase was balanced with the amount of lithium entering the vacancy of solid phase was balanced with the amount of lithium+ entering the vacancy of Al(OH) . The lithium Al(OH)3. The lithium recovery percentage and Li concentration in the filtrate we3re no longer recovery percentage and Li+ concentration in the filtrate were no longer increased. increased. . Figure 7. Lithium recovery percentage (round symbol) and Li+ concentration in the filtrate (triangle symbol) from LiAl-LDHs-1 at varied recovery temperatures of+65 ◦C, 75 ◦C, 85 ◦C, 95 ◦C. Figure 7. Lithium recovery percentage (round symbol) and Li concentration in the filtrate (triangle symbol) from LiAl-LDHs-1 at varied recovery temperatures of 65 °C, 75 °C, 85 °C, 95 °C. 27 In the NMR spectra (Figure S6A), the peaks corresponding to the chemical shift of Al in the solid productafterlithiumrecoverywere6.35,6.19,and6.07ppmat65◦C,75◦C,and85◦C,re2s7pectively. In the NMR spectra (Figure S6A), the peaks corresponding to the chemical shift of Al in the The main peak of the 27Al NMR spectra was 6 ppm at 95 ◦C, and a peak appeared with a relatively solid product after lithium recovery were 6.35, 6.19, and 6.07 ppm at 65 °C, 75 °C, and 85 °C, broad low-frequency shoulder at 12.729 ppm (Figure S6B) [37]. This phenomenon was consistent with respectively. The main peak of the Al NMR spectra was 6 ppm at 95 °C, and a peak appeared with a theliteraturewhereAl(OH) asgibbsitephasehadashoulderpeak[38].Withincreasingtemperature, relatively broad low-frequency shoulder at 1.29 ppm (Figure S6B) [37]. This phenomenon was 3 phase, where the amount of Li+ dissolved with consistent with the literature where Al(OH)3 as gibbsite phase had a shoulder peak [38]. With the solid product was transformed to the Al(OH) 3 Cl- from LiAl-LDHs-1 increased; in other words, the lithium recovery percentage increased. Through increasing temperature, the solid product was transformed to the Al(OH)3 phase, where the amount the li+thium recovery perce-ntage, the requirements of lithium recovery could be met at a temperature of Li dissolved with Cl from LiAl-LDHs-1 increased; in other words, the lithium recovery of 85 ◦C and 95 ◦C. Obviously, nearly the same effect was achieved at 95 ◦C and reduced energy percentage increased. Through the lithium recovery percentage, the requirements of lithium consumption was achieved at 85 ◦C. recovery could be met at a temperature of 85 °C and 95 °C. Obviously, nearly the same effect was achieved at 95 °C and reduced energy consumption was achieved at 85 °C. 3.4. Lithium Recovery Time 3.4. LTithieurmeaRceticonvetriymTeimdetermines the degree of the reaction. The XRD patterns (Figure S7) show that the LiAl-LDHs phase gradually disappears with increasing reaction time from 30 min to 120 min. The reaction time determines the degree of the reaction. The XRD patterns (Figure S7) show that After 90 min of reaction, a sharp and high-intensity Al(OH)3 characteristic diffraction peak appeared the LiAl-LDHs phase gradually disappears with increasing reaction time from 30 min to 120 min. with planes of (002), (110), (022), and (324). The effect of time on the lithium recovery percentage was After 90 min of reaction, a sharp and high-intensity Al(OH)3 characteristic diffraction peak appeared consistent with the temperature, as lithium recovery percentage increases with increasing reaction with planes of (002), (110), (022), and (324). The effect of time on the lithium recovery percentage was time. The reaction was essentially complete after 90 min because the lithium recovery percentage no consistent with the temperature, as lithium recovery percentage increases with increasing reaction longer increased (Figure 8). The Li+ concentration was 141.6 mg/L and 142.0 mg/L in the liquid phase time. The reaction was essentially complete after 90 min because the lithium recovery percentage no at 90 min and 120 min, respectively. No Al3+ dissolution was observed within the detection limit. longer increased (Figure 8). The Li+ concentration was 141.6 mg/L and 142.0 mg/L in the liquid phase Within the range of error, we consider that the Li+ concentration in the filtrate is the same with reaction at 90 min and 120 min, respectively. No Al3+ dissolution was observed within the detection limit. times of 90 min and 120 min. Within the range of error, we consider that the Li+ concentration in the filtrate is the same with reaction times of 90 min and 120 min.

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