Hydrotalcite-like compounds, also known as layered double hydroxides (LDH), from system Zn-Ni-Cu/Fe-Al/SO4 2- were obtained by co-precipitation at pH variable (increasing) using red mud (RM) as starting material due high contents of Fe3+ and Al3+. For this study, RM, previously characterized by XRF and XRD, was subjected to acid digestion with HClconc. and H2SO4 2N. For the LDHs obtained were evaluated influence of divalent cation, pH range of synthesis (pH 5, 7, 8, 9, 10 and 12) and the theoretical variation of molar ratio r = MII/MIII (2, 3 and 4) in the crystal structure using the characterization techniques: XRD, FT-IR, SEM/EDS, TGA/DTA. XRF revealed that RM is mainly composed of Fe2O3 (32.80%), Al2O3 (19.83%) SiO2 (18.14%) and Na2O (11.55%). XRD corroborates the results of chemical analysis, since the minerals were identified: hematite, goehtite, gibbsite, sodalite, calcite, quartz and anatase. Zn-LDHs showed that the increase in pH of the synthesis improves the crystalline order of the material, since the well-defined peaks become better culminating with the pH of synthesis set at pH 9, where LDH was identified as the natroglaucocerinite (d ~ 11 Ǻ). In these pH values, the incorporation of SO42- in the interlayer spacing was favored, despite competition with the CO2 present in atmospheric air at the synthesis time. FT-IR also indicates the presence of sulfate. Analysis by SEM showed very thin and small crystals, smaller than 2μm, that the hexagonal shape. Analysis by EDS showed its composition to the elements Na, Zn, Fe, Al, S, C and O. TGA/DTA analysis revealed the steps of dehydration, dehydroxylation, desoxygenation and desulfation. For the less crystalline materials, the first two occur simultaneously. Ni-LDHs showed three peaks with positions close to the mineral carrboydita from pH 7 to pH 12. However, from pH 9 at 12, there hematite as an accessory phase. Also there is dispute between the anions SO42- and CO32- in the interlayer space, whereas the values of basal spacing d decreases (approximately 9.5 to 7.8 Ǻ). This fact was also observed by FT-IR. Analysis by SEM showed agglomerates of anhedral minerals smaller than 2μm, presented by EDS composition Ni, Fe, Al, S, C and O. The analysis TGA/DTA shows the same previous behavior, showing the steps of dehydration, dehydroxylation, deoxygenation and desulfation and for the less crystalline materials, also the first two steps occur simultaneously. Cu-LDHs at pH values from 7 to 10, do not crystallize such that the LDH phase. Copper distorted octahedron structure causing Jahn-Teller effect: distorted tetrahedral in the octahedral. Analysis by FT-IR showed the same behavior as the previous samples, while the amorphous material is present. The SEM also shows that amorphous agglomerates according to the ESD, exhibit in their composition the elements Cu, Fe, Al, S, C and O. The analysis TGA/DTA exhibited the same behavior as the less crystalline materials of the two previous systems, for which dehydration and dehydroxylation steps occur simultaneously. Mt-LDHs (mixture of Zn2+, Ni2+, Cu2+), presented a similar behavior to Ni- LDHs, with four peaks at positions close to the carrboydita from pH 7 at 12. The dispute between sulphate and carbonate also repeated, since the basal spacing d values decrease (approximately 9.5 to 7.9 Ǻ), which can also be seen in the FT-IR spectra. The SEM samples showed these agglomerates with sizes smaller than 2μm, and EDS present in the composition elements Zn, Cu, Ni, Fe, Al, S, C and O. Here also the behavior of the TGA/DTA was similar to that obtained previously poorly crystalline materials.
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