Structural Study of Interlayer Zr Particles in Exchanged and Pillared Beidellite

Abstract
Zirconia pillared clays (with synthetic beidellite as host material) were prepared by replacing the sodium interlayer cations by zirconium hydroxy polycations, and then heating to stabilize the structure. The pillaring solution was an aqueous solution of zirconyl chloride, but the structure of the polycation which is intercalated remains unknown. From the XRD data. the interlayer spacing was found to be 9 Å in Zr exchanged beidellite and slightly lower (7Å) after calcination. The local environment of zirconium in solid zirconyl chloride and in the pillaring solution was first examined and then in the ion-exchanged and calcined beidellite. The EXAFS results for zirconyl chloride in the solid state and in aqueous solution, showed that the nearest neighbours and the next-nearest-neighbours environments of Zr are identical in solid and in solution. In the Zr-exchanged beidellite, the Zr cations have the same environment as in the pillaring solution. On the opposite. the mean Zr-O and Zr-Zr distances in the calcined sample are shortened with respect to Zr-exchanged beidellite.