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Molecules 2017, 22, 403 10 of 21 Figure 8. Response surfaces and contour plots for: (a) extraction time vs. pressure; and (b) extraction time vs. temperature. It was reproduced from reference [162] with permission from the Royal Society of Chemistry, 2014. 2.0 1.5 1.0 0.5 liq CO2 sc CO2 3.5 3.0 2.5 2.0 ACN ACN/PC (3:1) 1.5 DEC 1.0 0.5 0.0 0 10 20 30 40 50 60 Time [min] 0.0 0 5 10 15 20 Time [min] Figure 9. (Left) Time dependency of the amount of recovered electrolyte from commercial 18,650 cells after formation extracted with supercritical (300 bar, 40 °C; red stars) and liquid (60 bar, 25 °C; black squares) CO2; and (Right) time dependency of the amount of recovered electrolyte from commercial 18,650 cells after formation extracted with liquid CO2 and 0.5 mL/min additional solvents (black stars: acetonitrile (can); magenta triangles: ACN/propylene carbonate (PC) (3:1); red circles: diethyl carbonate (DEC)). It was reproduced from reference [163] with permission from the Royal Society of Chemistry, 2015. 4.0 3.5 (3.17 ± 0.21) g 3.0 (3.35 ± 0.13) g (3.76 ± 0.19) g 18650 reference (3.03 ± 0.06) g 2.5 2.0 1.5 1.0 0.5 0.0 ACN DEC ACN/PC (3:1) Figure 10. Compositions and amounts (determined with gas chromatography—mass spectrometry (GC-MS) and ion chromatography (IC)) of the recovered electrolytes from commercial 18,650 cells after formation extracted with liquid CO2 and additional solvents for 30 min, with subsequent 20 min without additional solvent. Red, top: LiPF6; blue, below: ethylene carbonate (EC); yellow, middle: ethyl methyl carbonate (EMC); magenta, bottom: dimethyl carbonate (DMC). It was reproduced from reference [163] with permission from the Royal Society of Chemistry, 2015. LiPF6 Recovered electrolyte [g] Recovered electrolyte [g] Recovered electrolyte [g]PDF Image | CO2 for Recycling and Sample Preparation of Lithium Ion Battery
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