Preparation of Porous Silica-Pillared Layered Phase:  Simultaneous Intercalation of Amine-Tetraethylorthosilicate into the H⁺-Magadiite and Intragallery Amine-Catalyzed Hydrolysis of Tetraethylorthosilicate

Porous silica-pillared H + -magadiites were prepared by intragallery amine-catalyzed hydrolysis of TEOS [tetraethylorthosilicate, Si(OC 2 H 5 ) 4 ]. Mixtures of the H + -magadiite, dodecylamine, and TEOS at molar ratios of 1:2:15−30 and 1:2−10:20 resulted in swollen and viscous gel once at room temperature, allowing intercalation compounds in which dodecylamine and TEOS were simultaneously intercalated into interlayers of H + -magadiite. The hydrolysis of the gallery TEOS was conducted in water solution for 40 min at room temperature, affording siloxane-pillared H + -magadiites with a gallery height of between 30.2 and 39.2 Å. Calcination of samples at 538 °C in air resulted in silica-pillared magadiites with large specific surface areas between 607 and 830 m 2 /g, depending on the reaction stoichiometry. The reaction at H + -magadiite:dodecylamine:TEOS reaction stoichiometries of 1:2:15 and 1:6:20 resulted in optimum specific surface areas and mesopores with a narrow pore size distribution. Result indicates that the intragallery amine catalyzes the hydrolysis of gallery TEOS and simultaneously has a role of gallery-templated micellar assemblies.