Synthesis and characterization of a hexagonal mesoporous silica with enhanced thermal and hydrothermal stabilities

Abstract

A synthetic route was developed for a novel hexagonal mesoporous silica that has remarkably wide channel diameters and thick walls. The procedure involved the acid-catalyzed hydrolysis of tetraethylorthosilicate in a water/ethanol/isopropoanol solvent mixture while employing 1-hexadecylamine as a templating agent and mesitylene as an auxiliary agent. After removal of the template by either extraction with ethanolic hydrochloric acid or by calcination at 550 °C, the resulting mesoporous materials had surface areas of 1283 and 1211 m 2 /g. The channel diameters were found to be 47.2-51.1 Å, while the wall thicknesses were 20.9-21.1 Å. X-ray powder diffraction demonstrated that the novel mesoporous silica belonged to the MCM-41 structural family. Notably, they displayed higher thermal and hydrothermal stabilities, and have higher surface areas than conventionally prepared MCM-41 silica. The thickest channel walls (21.1 Å) can withstand calcination to nearly 850 °C with minimal structural damage. The calcined sample was more resistant to hydrothermal treatment in boiling water than was the solvent-extracted product but both materials showed minimal change after 25 h of hydrothermal treatment. © 2010 Elsevier B.V.