In this study, mesoporous nanocomposite silicotungstic acid (STA) incorporated MCM-41 and mesoporous aluminosilicate catalysts with narrow pore size distributions, in the range of 2.5-3.5 nm, were successfully synthesized following different impregnation procedures. Results showed that the catalyst preparation procedure had significant influence on its activity as well as the product distribution in ethanol dehydration. STAMCM41C catalyst, which was prepared by the impregnation of STA into calcined MCM-41 containing a W/Si ratio of 0.24, and STAMAS catalyst, which was prepared by the impregnation of STA into mesoporous aluminosilicate, showed very high activities in dehydration of ethanol. Ethylene yield showed an increasing trend with temperature, reaching to about 100% above 250 °C. In contrast to ethylene, DEE was formed at lower temperatures, reaching to a yield value of about 70% at 180 °C with STAMCM41C. DEE formation at lower temperatures was concluded to be due to the presence of Bronsted acid sites of this catalyst. © 2008 American Chemical Society.