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Molecules 2017, 22, 403 9 of 21 plasma–optical emission spectrometry (ICP-OES) were applied to systematically investigate the extract. The final recovery rate was determined as 85.07% ± 0.36%, however the conducting salt could not be recovered in sufficient amounts. They proposed that LIPF6 was hydrolyzed during the supercritical CO2 extraction process extraction, which was investigated with NMR to observe typical PF6− hydrolysis products. Furthermore, the extraction parameters were optimized by varying the operating parameters (extraction pressure, temperature and static time) according to the Box–Behnken design (Figure 8). With the help of a polynomial regression model, the mildest experimental conditions were determined (23.4 MPa, 40 °C and 45 min). The predicted recovery rate, 85.22%, was in very good agreement with the experimental recovery rate of 85.07%. Additionally, the results of the experiment showed that the extraction pressure is the major decisive factor for electrolyte extraction. Figure 7. Schematic setup of the applied extraction procedure by Dai et al. with (1) CO2 cylinder; (2) cooling bath; (3) air driven fluid pump (gas booster pump); (4) air compressor; (5) air regulator; (6) CO2 pressure; (7) inlet valve; (8) extraction vessel; (9) heating jacket; (10) vessel heat; (11) vent valve; (12) outlet valve; (13) flow valve; (14) valve heat; (15) heating jacket; (16) collecting vial; (17) alumina filter; and (18) gas flow meter. It was reproduced from reference [162] with permission from the Royal Society of Chemistry, 2014. In agreement with Grützke et al. [19], they emphasized the usefulness of supercritical CO2 as an efficient and environment-friendly electrolyte separation method. Following their static experiments, Grützke et al. applied a flow-through design [163]. They used supercritical and liquid carbon dioxide (sc and liq CO2) under addition of different solvents for the optimized extraction of the electrolyte from commercial LiNi0.33Co0.33Mn0.33O2 (NMC))/graphite 18,650 cells (Figure 9). With 89.1 ± 3.4 wt %, the best overall recovery rate was achieved for the added ACN/PC mixture with the highest concentrations for EC and LiPF6 (Figure 10). In addition, they investigated the time dependency of the recovered electrolyte for both setups. It was demonstrated that the developed method was suitable for LIB electrolyte extraction and post-mortem or aging investigations of LIB cell components because a qualitative overview was achieved after a few minutes of extraction also for apparently “dry” cells, where the electrolyte is deeply incorporated and immobilized in the electrode material.PDF Image | CO2 for Recycling and Sample Preparation of Lithium Ion Battery
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