In this experimental study, the alkali activation of acid leaching residues using a mixture of sodium hydroxide (NaOH) and alkaline sodium silicate solution (Na2
) as activators is investigated. The residues were also calcined at 800 and 1000 °C for 2 h or mixed with metakaolin (MK) in order to increase their reactivity. The effect of several parameters, namely the H2
O and SiO2
O ratios present in the activating solution, the pre–curing time (4–24 h), the curing temperature (40–80 °C), the curing time (24 or 48 h), and the ageing period (7–28 days) on the properties of the produced alkali activated materials (AAMs), including compressive strength, porosity, water absorption, and density, was explored. Analytical techniques, namely X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and elemental mapping analysis were used for the identification of the morphology and structure of the final products. The experimental results show that the laterite acid leaching residues cannot be alkali activated in an unaltered state, and the compressive strength of the produced AAMs barely reaches 1.4 MPa, while the mixing of the residues with 10 wt% metakaolin results in noticeably higher compressive strength (41 MPa). Moreover, the calcination of residues at 800 and 1000 °C has practically no beneficial effect on alkali activation. Alkali activated materials produced under the optimum synthesis conditions were subjected to high temperature firing for 2 h and immersed in distilled water or acidic solution (1 mol L−1
HCl) for 7 and 30 days in order to assess their structural integrity under different environmental conditions. This study explores the potential of alkali activation of laterite leaching residues amended with the addition of metakaolin for the production of AAMS that can be used as binders or in several construction applications in order to enable their valorization and also improve the environmental sustainability of the metallurgical sector.
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