Mesoporous aluminosilicate in the hexagonal phase (MCM-41) has been synthesized from fusedfly ash solutions and cationic cetyltrimethylammonium bromide (CTAB) surfactants. We providedirect evidence that an MCM-41 aluminosilicate with a homogeneous chemical composition ofSi/Al = 13.4 can be prepared with cationic surfactant. Our results indicate that coal combustionbyproducts can be utilized for producing mesoporous molecular sieves even though they containsignificant amounts of impurities.