The Keggin-ion [SiW11(TiO2)O39]^6^-, [SiW9(TiO2)3O37]^-^1^0, [PW11(TiO2)-O39]^5^-, [PW9(TiO2)3O37]^9^- intercalated Zn2Al hydrotalcite-like compounds were prepared by means of direct ion-exchange reaction in aqueous solution, and were characterized by elemental analysis, XRD, IR and XPS spectra. The interlayer space of the pillared products increased from 0.92nm to 1.47nm with the peroxoheteropolyanions displacing the NO3^- ions in the gallery. Results from IR and XPS show that the peroxoheteropolyanions structure are well remained. The pillared products showed good catalytic behavior over the cyclohexene conversion.

Key words: INFRARED SPECTROPHOTOMETRY, ELEMENTAL ANALYSIS, X-RAY DIFFRACTION ANALYSIS, ION EXCHANGING, SILICON COMPOUNDS, X-RAY PHOTOELECTRON SPECTROMETRY, CYCLOHEXENE, PHOSPHORUS COMPOUNDS, TUNGSTEN COMPOUNDS, HYDROTALCITE