Siliceous mesoporous materials with pores of ordered 2-D hexagonal structure were successfully prepared without hydrothermal treatment from condensation-polymerization of various concentration of quaternary ammonium salt as structure directing agents and silica precursor from the supernatant of coal fly ash (CFA) in the presence of catalyst. The synthesized materials had high surface area of ca. 740 m(2) g(-1) and pore volume of ca. 0.42 mL g(-1). The synthesized material exhibited a narrow size pore distribution and the mean pore diameter as measured by Dollimore-Heal method was about 2.3 nm. The formation of ammonium salt that act as precipitant during the synthesis enable the hydrolysis and co-condensation of the sodium silicate at room temperature. (c) 2006 Elsevier B.V. All rights reserved.