This study investigated the gaseous products evolution behaviors and the recovery performance of cathode materials from spent LiFePO 4 batteries by vacuum pyrolysis. The thermogravimetric-differential scanning calorimetry analysis coupled with electron ionization mass spectrometry (TG-DSC-EI-MS) results indicated that inorganic gases (H 2 O, CO, CO 2 ), alkane gases (CH
In this study, the effects of oxidizing roasting process on the liberation of cathode materials from Al foil under different conditions were investigated systematically. The mineralogical characteristics of the cathode materials before and after thermal treatment were extensively characterized using scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) as well as Fourier transform infrared (FT-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS). The results indicated that the increase in roasting temperature, oxygen concentration, and air flow rate enhanced the liberation of cathode materials. The cathode materials were gradually oxidized to Li3Fe2(PO4)3 and Fe2O3. Further, the carbon and fluorine content in the cathode materials decreased slowly during the thermal treatment, while the Al content increased. When the roasting temperature exceeded the melting point of Al, the Al foils were ablated and the cathode materials adhered to the Al foils again, resulting in difficulty in separation. The cathode materials leaching performance test results demonstrated that the oxidation of cathode materials had a negative effect on the leaching of Fe in sulfuric acid leaching system.
The leaching kinetics of hemimorphite (Zn 4 Si 2 O 7 (OH) 2 •H 2 O) in ammonium chloride solution was presented in detail. Effects of stirring speed (150-350 rpm), leaching temperature (75-108 • C), particle size of hemimorphite (45-150 µm), and the concentration of ammonium chloride (3.5-5.5 mol/L) on the zinc extraction rate were studied. The zinc extraction rate enhanced slightly with the increase in stirring speed, but increased significantly with an increase in the leaching temperature and ammonium chloride concentration. Zinc extraction was enhanced significantly in the first 60 min with decreasing particle size, but had little effect on the leaching process after 60 min. Scanning electron microscopy (SEM) analysis showed that some silica gel formed in the leaching process was not separated from the hemimorphite surface, but covered some of the active particle surface. The Elovich equation successfully described the leaching kinetics of hemimorphite in ammonium chloride solution with an apparent activation energy of 405.14 kJ/mol at temperatures of 75-90 • C and 239.61 kJ/mol at temperatures of 95-108 • C, which is characteristic for a chemically-controlled process. Silica gel is generated at temperatures of 75-90 • C and decomposed into silica at temperatures of 95-108 • C.
In this research, some experimental steps were investigated to recover zinc contained in crude zinc oxide (C.Z.O.). In the first stage, the C.Z.O. was treated in NH3–NH4Cl–H2O solution to dissolve the metals. The optimized leaching conditions in batch experiments were obtained: agitation speed 250 rpm, concentration of ammonia and ammonium chloride 2.5 mol/L and 5 mol/L, respectively, time 30min, temperature 40 °C, and L/S = 6 mL/g. The extraction percentage of zinc was over 81% under the optimized leaching conditions. The kinetic study indicates that zinc extraction from the C.Z.O particles was very rapid. In the second stage, the solution from the leaching process was purified by adding zinc dust to the solution. The Cu, Cd, Pb, Sb, and As could be reduced to levels of 0.03, 0.09, 0.87, 0.22, and 0.12 mg/L after the purification process. Finally, the electrowinning process was used to recover dissolved Zn from the final solution. The zinc content in the electrowon zinc was more than 99.99%.
The leaching behavior of hemimorphite in neutral solution (NH4 +-Cl--H2O) was investigated at high temperature (T > 100?C) under a range of experimental conditions. Thermodynamic calculations indicate that the tendency of dehydration of silica gel is significantly enhanced with the increasing temperature. It was shown that the temperature, ammonium chloride concentration, or L/S ratio increased resulted in greater leaching efficiency. The following optimized leaching conditions were obtained: stirrer speed 400r/min, NH4Cl concentration 5.5M, L/S ratio 9mL/g at 160?C for 3h. Under these optimized conditions, the average leaching yield of zinc was 97.82%. The silicon was converted to quartz and remained in the residue. This process can be used to dispose willemite and hemimorphite as it solves the problem of silica gel dehydration.
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