Mesoporous materials containing aluminum and titanium were obtained by direct synthesis at room temperature, using a sol-gel method with two reaction steps (acid and alkaline hydrolysis). After solvent extraction and calcination (550 ºC), the solids were labeled as H-MCM-41, Al-MCM-41(10), Al-MCM-41(30) and Ti-MCM-41(40). The numbers in parenthesis denote the Si/metal molar ratio of the structure. A hexagonal mesoporous silica containing titanium, Ti-HMS(30), was also prepared, using primary dodecylamine as a template at pH 10. The total preparation time in both procedures was less than 17 h, including an aging phase in the synthesis liquor. The net synthesis yields were higher than 40 %, which makes this method very promising. Characterization of samples were made by infrared spectroscopy, thermogravimetry, X-Ray diffraction, N2 adsorption at 77K, light scaterring, XPS spectroscopy, and measurements of surface acidity and chemical analysis (ICP, EDX). The adsorptive properties of the H-MCM-41 and aluminosilicate samples for polyaromatics hydrocarbons (naphtalene, anthracene and pyrene) were also studied at 25, 40 and 60 ºC. The best adsorption capacity was obtained for pyrene in Al-MCM-41(10), with a value of 1.83 mmol/g. For the aluminosilicates, the adsorption capacity is slightly influenced by the amount of incorporated Al. In general, the results confirm that the synthesized materials are promising catalysts (redox and acids), catalytic supports and adsorbents.