The synthesis of some mesostructured silica or aluminosilica SBA-16 and Al-SBA-16 with 3D cubic structure is reported in this paper. The structural and porosity properties of these materials were studied by XRD, N-2 sorption and TEM imaging; the Al insertion was determined by Al-27-MAS-NMR and acidic properties were characterized by pyridine adsorption followed by FT-IR spectroscopy. These solids were tested in the selective catalytic reduction of NOx by ethanol in the presence of O-2. Compared to hexagonal mesoporous silica or aluminosilica (SBA-15 and Al-SBA-15), SBA-16 type materials (SBA-16 and Al-SBA-16) could be used as potential catalyst for the oxidation reaction and the SBA-16 solid has higher catalytic properties for the reduction of NOx to N-2 at high temperature.