Recovering iron from the bauxite residue (BR) is one of the long-standing challenges in the mining industry. However, there is a substantial lack of information in the literature regarding sample properties and iron extraction by reducing hydrogen. The present study aims at reducing a Greek BR using hydrogen, its characterization, and separating iron by magnetic separation processes. To this end, the reduced sample was characterized using X-ray diffractometry analysis (XRD), X-ray fluorescence spectrometer analysis (XRF), thermomagnetic analysis (TMA), automated mineralogy (AM), and scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS). The effect of particle size (−200 + 100 µm, −100 + 75 µm, and <75 µm) was investigated through a medium-intensity magnetic separation (MIMS, Davis Tube) at 1000–2500 Gauss and a Slon® magnetic separator (1000 G). The effects of solid content (3% and 10% w/w) in a wet low-intensity magnetic separation (WLIMS, 350 G) and a two-stage MIMS followed by WLIMS were investigated. It was revealed that through reduction at 500 °C and 2 h with 20 wt% NaOH under 5 vol.% H2 + 95 vol.% N2, iron oxides and ferric oxyhydroxide (Fe2O3 and FeOOH) were converted into magnetite (Fe3O4), whereas aluminum (oxy)hydroxides (Al(OOH), Al(OH)3) were reacted with Na+ towards sodium aluminates (NaAlO2). The AM observations indicated that only 3% of iron was in the phase of liberated magnetite, and the remaining was associated with Na, Al, and Ti phases with different intensities. The dissemination of iron throughout the matrix of the sample was recognized as the principal challenge in the physical separation processes. It was found that increasing magnetic intensity from 1000 G to 2500 G resulted in improved recovery for all studied particle size fractions in Davis Tube tests. The particle range of −106 + 74 µm was chosen as the most appropriate size to achieve the maximum Fe content of 41%. The results of WLIMS (350 G) showed the maximum Fe grade but revealed less recovery of 52% and 27% at 10% and 3% solid contents, respectively, compared to the Davis Tube trials.

Experimental research was carried out to produce pellets from bauxite residue for the further extraction of iron and alumina. Bauxite residue and limestone with three different mixture compositions were pelletized experimentally via agglomeration followed by drying and sintering at elevated temperatures. X-Ray diffraction (XRD) and scanning electron microscopy (SEM) were used for the phase and microstructural analysis, respectively. Tumble, abrasion, and breaking load tests were applied to determine the strength of the pellets. For measurement of porosity and surface area, mercury porosimetry and BET surface area methods were applied. It was found that at 1100 °C sintering temperature, all the three sintered pellet compositions have a moderate porosity and low strength, but the reverse result was found when 1200 °C sintering temperature was applied. Moreover, for the pellets sintered at 1150 °C high strength and proper porosities were obtained. In the sintered pellets, iron present in form of brownmillerite (Ca2Fe1.63Al0.36O5), srebrodolskite (Ca2Fe2O5), and fayalite (Fe2SiO4), while alumina present mostly in gehlenite (Ca2Al2SiO7) and little fraction in mayenite (Ca12Al14O33) and brownmillerite phases. The identified phases are the same for of the three pellets, however, with variations in their quantities. Porosity and mechanical properties of pellets are inversely related with both varying sintering temperature and composition. It was found that with more CaCO3 use in pelletizing, higher porosity is obtained. However, with increasing sintering temperature the strength of the pellets increases due to clustering of particles, while porosity decreases.

In this study, the isothermal reduction of bauxite residue-calcite sintered pellets by hydrogen at elevated temperatures and different gas flow rates was investigated. A thermogravimetric technique was applied to study the kinetics of the direct reduction by H2 at 500–1000 °C. It was observed that iron in sintered oxide pellets mainly exists in the form of brownmillerite, srebrodolskite and fayalite. The reduction of brownmillerite, the dominant Fe-containing phase, with hydrogen produces mayenite, calcite and metallic iron. X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray fluorescence (XRF), BET surface area, pycnometer and mercury intrusion porosimeter analyses were adopted on reduced pellets to interpret the experimental results. The order of the reduction process changes from first-order reaction kinetics to second-order with an increasing reduction temperature. The change in reaction order may be due to sintering at higher reduction temperatures and corresponding physical and microstructural changes in pellets. The activation energy of reduction was calculated as 55.1–96.6 kJ/mol based on the experimental conditions and using different kinetic model equations. From the experimental observations, it was found that 1000 °C with 60 min is the most suitable condition for bauxite residue-CaO sintered pellets’ reduction with hydrogen.

This study investigates the properties of H2-reduced calcium-added bauxite residue, self-hardened pellets, and the feasibility of iron recovery through electrostatic and magnetic separation methods. The oxide pellets are prepared via a mixing of bauxite residue, calcite, and quicklime. The self-hardened pellets are reduced at 1000 °C with hydrogen gas flow for 120 min. The chemical composition, phase identification, and microstructural observations are executed using X-ray fluorescence (XRF), X-ray diffraction (XRD), and scanning electron microscopy (SEM), respectively. The porosity and strength of the self-hardened pellets are performed by the Mercury intrusion porosimetry and tumbling tests, respectively. The separation of iron is examined through a dry electrostatic technique, and in wet conditions, i.e., via Davis Tube and low-intensity magnetic separation (WLIMS). The effect of the magnetic field (0.1, 0.25, and 0.32 T) is tested on two different particle size fractions (−212 + 106 µm and −106 + 74 µm). It is found that most of the iron oxide in the bauxite residue is converted to metallic iron, which corresponds well with both XRD and SEM results. The Carpco electrostatic tests indicate that this approach is inefficient for the studied type of material because of the intensive association of iron with the rest of the components leading to transferring it to the middling rather than to conductive product. However, both the Davis Tube and WLIMS approve a reasonable improvement in the Fe content from 22% to 37% with acceptable recoveries. The results of the Davis Tube show that there is an optimum magnetic field and particle size for maximization of Fe grade and recovery. Finally, further suggestions are highlighted for the physical beneficiation of studied bauxite residue with the purpose of maximizing iron grade and recovery.

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