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

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Abstract

Porous silica-pillared H+-magadiites were prepared by intragallery amine-catalyzed hydrolysis of TEOS [tetraethylorthosilicate, Si(OC2H5)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 m2/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.

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