Oxidative roasting of Nd-Fe-B permanent magnets prior to leaching improves the selectivity in the recovery of rare-earth elements over iron. However, the dissolution rate of oxidatively roasted Nd-Fe-B permanent magnets in acidic solutions is very slow, often longer than 24 h. Upon roasting in air at temperatures above 500 °C, the neodymium metal is not converted to Nd 2 O 3 , but rather to the ternary NdFeO 3 phase. NdFeO 3 is much more difficult to dissolve than Nd 2 O 3. In this work, the formation of NdFeO 3 was avoided by roasting Nd-Fe-B permanent magnet production scrap in argon atmosphere, having an oxygen content of p O 2 ≤ 10 −20 atm, with the addition of 5 wt% of carbon as an iron reducing agent. For all the non-oxidizing iron roasting conditions investigated, the iron in the Nd-Fe-B scrap formed a cobalt-containing metallic phase, clearly distinct from the rare-earth phase at microscopic level. The thermal treatment was optimized to obtain a clear phase separation of metallic iron and rare-earth phase also at the macroscopic level, to enable easy mechanical removal of iron prior to the leaching step. The sample roasted at the optimum conditions (i.e., 5 wt% carbon, no flux, no quenching step, roasting temperature of 1400 °C and roasting time of 2 h) was leached in the water-containing ionic liquid betainium bis(trifluoromethylsulfonyl)imide, [Hbet][Tf 2 N]. A leaching time of only 20 min was sufficient to completely dissolve the rare-earth elements. The rare-earth elements/iron ratio in the leachate was about 50 times higher than the initial rare-earth elements/iron ratio in the Nd-Fe-B scrap. Therefore, roasting in argon with addition of a small amount of carbon is an efficient process step to avoid the formation of NdFeO 3 and to separate the rare-earth elements from the iron, resulting in selective leaching for the recovery of rare-earth elements from Nd-Fe-B permanent magnets.
In Europe, 50% of the copper originates from recycling. High-Cu containing scraps are regularly rich in impurities like Fe, Ni, Sn and Pb. Many high-Cu containing scraps are fed directly into anode-furnace casting installations or furnaces with limited refining capability. The impurities levels of the anodes produced in these processes should however remain acceptable for further electro-refining. The distribution of Sn between copper and slag has been investigated for conditions relevant to copper converting. Unlike previous studies, this work focuses on the behavior of Sn relevant to fire refining conditions, which are essential for anode refineries.In this study, liquid Cu-1Sn and CuO x-FeO y-SiO 2 slag, with CaO additions, were equilibrated at 1300°C in vacuum sealed SiO 2 ampoules. After metal-slag equilibration, the samples were quenched in water. The composition of the slag and Cu metal was investigated with Electron Probe X-ray Microanalysis. The distribution coefficients of Sn between slag and Cu metal were determined as a function of slag composition.
The goal of this work is to accurately measure the viscosity of an industrial secondary copper smelting slag. Established literature commonly performed such measurements in non-inert labware, such as alumina. Despite the fact that the dissolution of alumina into the slag was addressed as a source for errors, a comprehensive analysis of how this interaction affects the measurement reliability is hitherto lacking. Furthermore, the type of dissolution (direct or indirect) will influence the interaction kinetics. This work aims to verify a possible relation between the dissolution and viscosity measurement reliability. For this purpose, the infiltration depth during and time stability of four different slag (PbO-SiO 2 -CaO-Al 2 O 3 -ZnO-Fe 2 O 3 ) viscosity measurements were analyzed. Both in-situ viscosity measurements and post mortem SEM images of the interface were therefore analyzed. It was observed that a multiphase interfacial layer was formed upon alumina dissolution. This layer consisted of a spinel intermediate layer and an enclosed interfacial slag. EDX measurements confirmed the difference between the latter layer's composition and the bulk slag. Samples with a high interfacial slag viscosity yielded a dense spinel layer. As a result, alumina dissolved indirectly and more reliable viscosity measurements were obtained that were more stable over time. While samples with a low interfacial slag viscosity yielded a discontinuous spinel layer and therefore alumina could dissolve fast into the bulk slag, resulting in more unreliable viscosity measurements that varied over time.
A systematic isothermal reduction study was carried out on pure PbO pellets using 15 pct H2/85 pct N2 gas. The reduction was carried out at 350 °C to 800 °C at different reaction times (30 minutes to 4 hours) with gas flowrate of 500 mL/min. The kinetics of the reaction were evaluated by measuring the mass change and applying kinetic models to the data. The results from microstructure observation showed that globular and non-wetting lead droplets form on the surface of PbO samples. The droplet's diameter was observed to increase with increasing temperature and reduction time. It was observed that this lead droplets layer, once covers the whole surface, appears to reduce the overall reduction rate. The kinetics analysis showed that PbO pellet reduction is a diffusion-controlled process as supported by the SEM (scanning electron microscope) micrographs, samples’ cross-section observation, and phase analyses using EDS (energy-dispersive spectrometry) and XRD (X-ray diffraction). The energy activation, Ea, was calculated for two temperature ranges, i.e., 61 kJ/mol (for 350 °C to 450 °C) and 224 kJ/mol (for 600 °C to 800 °C), respectively. These results suggest that, in an industrial context, continued reduction process will require constant removal of lead product from the surface of the lead monoxide.
The common procedure to calculate vapour-liquid equilibrium (VLE) from an ideal gas and activity coefficient model is evaluated. The reliability of these calculations is assessed through a quantification of the uncertainty in the thermodynamic data of Ag-Pb and Au-Pb binary alloys and propagation of this uncertainty in the calculation of a prediction interval for the vapour-liquid equilibrium results. The advantage of this methodology is that all calculated results include an uncertainty interval, which permits an assessment of the impact of the uncertainty in the thermodynamic data and allows for the validation of VLE diagrams with experimental data to be done on a quantitative basis.
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