Several heterogeneous catalysts based on MCM-41 were synthesized either by chemical vapor deposition (CVD) or hydrothermally, i.e. adding SnCl 4 , SnCl 2 or ZnCl 2 as precursor salts into the MCM-41 synthesis gel. Synthesized materials were characterized by XRD, BET surface area, atomic absorption, UV-Vis, H 2-TPR, NH 3-TPD, TEM and pyridine-FTIR. Better textural properties and more reactive materials were obtained using tin salt precursors compared with ZnCl 2. UV-Vis and TPR analyses of selected Sn-MCM-41 materials indicate that depending on the synthesis and pretreatment conditions several species may be formed: Sn 4+ as Lewis acid sites of different coordination, SnO 2 nanoparticles and bulk tin oxide species. The presence of SnO 2 nanoparticles was also confirmed by TEM. Medium strength Lewis acid sites appear to increase nopol selectivity. Hydroxylated groups, i.e. Sn-OH, increased the weak acid sites and diminished nopol selectivity.