The layered material Rb x Mn x Ti 2-x O 4 (x ) 0.75) was pillared with silica. The Rb ions were first exchanged with n-alkylammonium ions (C n H 2n+1 NH 3 , n ) 6-18) to separate the interlayer space of the titanate, and then tetraethoxysilane was hydrolyzed between the layers. Burning off the organic parts resulted in silica pillared microporous solids with a surface area as large as 500-800 m 2 /g. The porous structure was stable up to 600 °C. Adsorption-desorption isotherms for various vapors, such as water, methanol, toluene, and mesitylene, were measured, which suggested that the porous structure formed between the layers was very similar to those of zeolites and uniform without mesopores. The pores showed hydrophobic properties. Their size was on the order of that of mesitylene.

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