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Here, using liquid crystals as template, an EISA (evaporation-induced self-assembly) method has been used to synthesize amorphous mesostructured alumina. The effect of the synthesis parameters such as the presence of a chelating agent, the amounts of both porogen agent and alumina precursor on the materials properties have been investigated in details. Under the optimum conditions, after Soxhlet extraction, the obtained Al 2 O 3 presents an HMS (Hexagonal Molecular Sieves) structure and a high specific surface area (≈400 m2/g) with a mesopore size distribution centered around 8.3 nm. Investigation of the thermal stability shows that the crystallization into γ-Al 2 O 3 of the amorphous alumina walls delimiting mesopores begins after heating at 800 °C. We have also demonstrated that half of the carbon present in the as-synthesized material can be removed by washing with water or ethanol at room temperature instead of Soxhlet extraction. On the basis of SAXS, XRD and N 2 adsorption-desorption analyses, we have shown that when treated into boiling water or exposed to water vapor the alteration of the mesostructure occurs quickly. Its collapse has been attributed to the crystallization of the amorphous alumina walls into aluminum hydroxides, mainly boehmite, upon the hydration of the alumina. Dual mesoporous alumina have been also obtained from micelles through a cooperative templating mechanism at low P123 amount and in the presence of citric acid. In that case both mesopores networks adopt a wormhole-like mesostructure. [Display omitted] • Mesostructure preserved until 900 °C. • Amorphous mesostructured Al 2 O 3 thermally stable up to 800 °C. • Porogen agent partially removed by water or ethanol at room temperature. • Framework collapses due to aluminum hydroxides crystallization in presence of water. • Dual mesoporous alumina prepared at low amount of porogen agent in presence of citrate. [ABSTRACT FROM AUTHOR]