Physicochemical characterization and surface acid properties of mesoporous [Al]-SBA-15 obtained by direct synthesis

In this work, [Al]-SBA-15 samples were prepared by three different direct synthesis methods and one postsynthesis procedure, aiming to study the influence of the preparation procedures on their structural, textural, and physicochemical features. To this aim, samples were investigated by combining different experimental techniques (XRD, N(2) physisorption, (27)Al-MAS NMR, and IR spectroscopy). All preparation methods led to the formation of aluminum-containing SBA-15 samples. Nevertheless, depending on the preparation procedure, samples exhibited different structural, textural, and surface characteristics, especially in terms of Brønsted and Lewis acid sites content. [Al]-SBA-15(1) was synthesized by the pH-adjusting method and presented the lowest surface area and pore volumes. Its surface displayed three families of medium and one family of high strength Brønsted acid sites. The Brønsted/Lewis ratio was 3.49. [Al]-SBA-15(2) and [Al]-SBA-15(3) were synthesized by prehydrolysis of the silica and the aluminum precursors. In [Al]-SBA-15(2), ammonium fluoride was used as silica condensation catalyst. These two materials presented similar surface area, pore diameters and volumes, and Brønsted acidity. The Brønsted/Lewis acid sites ratio were 3.07 and 2.15 for [Al]-SBA-15(2) and [Al]-SBA-15(3), respectively. The [Al]-SBA-15(P) obtained by postsynthesis alumination displayed surface area similar to that of [Al]-SBA-15(3), Brønsted/Lewis acid sites ratio of 2.75, and Brønsted acidity similar to that of [Al]-SBA-15(1). The presence of extra-framework aluminum oxide was identified only on [Al]-SBA-15(3) and [Al]-SBA-15(P).