Ti(IV) polycation-intercalated niobate was synthesized through a stepwise ion-exchange route, in which HNb3O8 was used as the layered host, n-decylamine as a preswelling agent, and tetrabutyl titanate (abbreviated to TBT) as a titanium source. After the Ti(IV) polycation-intercalated niobate was calcined at 723 K in air environment, TiO2-pillared HNb3O8 was given. X-ray diffraction (XRD), framework infrared spectra FT-IR, N2 adsorption-desorption technique and transmission electron microscopy (TEM) were employed to investigate the structure of the obtained products. Characterizations by XRD and N2 adsorption-desorption isotherms indicated that the TiO2-pillared HNb3O8 was a porous layered material with an interlayer distance (d010) of 1.39 nm, a pillar height of 0.63 nm and a BET specific surface area of 35 m2•g－1. The TiO2-pillared solid was thermally very stable, and its layered structure could be retained up to 823 K. Combined with our previous studying work, it was found that TBT as well as titanium tetraisopropoxide (abbreviated as TIP) could be used as the precursor of TiO2 pillars. Apparently, the TBT is more practicable than TIP since the latter is very costly and the former relatively cheap. It was demonstrated that the Ti(IV) polycation intercalated in the interlayers of the layered niobate contain no CH3COO－ and other organic groups, and thus it can be inferred that the Ti(IV) polycations have a formula of [Ti(OH)x(H2O)y]z＋, in which x, y, and z are variables.

Key words: TiO₂-pillared HNb₃O₈, pillaring, titanium source, tetrabutyl titanate