Preparation of porous silica-pillared layered phase: Simultaneous intercalation of amine-tetraethylorthosilicate into the H+-magadiite and intragallery amine-catalyzed hydrolysis of tetraethylorthosilicate
Oy. Kwon et al., Preparation of porous silica-pillared layered phase: Simultaneous intercalation of amine-tetraethylorthosilicate into the H+-magadiite and intragallery amine-catalyzed hydrolysis of tetraethylorthosilicate, CHEM MATER, 12(5), 2000, pp. 1273-1278
Porous silica-pillared H+-magadiites were prepared by intragallery amine-ca
talyzed hydrolysis of TEOS [tetraethylorthosilicate, Si(OC2H5)(4)] Mixtures
of the H+-magadiite, dodecylamine, and TEOS at molar ratios of 1:2:15-30 a
nd 1:2-10:20 resulted in swollen and viscous gel once at room temperature,
allowing intercalation compounds in which dodecylamine and TEOS were simult
aneously intercalated into interlayers of H+-magadiite. The hydrolysis of t
he gallery TEOS was conducted in water solution for 40 min at room temperat
ure, affording siloxane-pillared H+-magadiites with a gallery height of bet
ween 30.2 and 39.2 Angstrom. Calcination of samples at 538 degrees C in air
resulted in silica-pillared magadiites with large specific surface areas b
etween 607 and 830 m(2)/g, depending on the reaction stoichiometry. The rea
ction 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 amin
e catalyzes the hydrolysis of gallery TEOS and simultaneously has a role of
gallery-templated micellar assemblies.