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Zirconium-containing mesoporous silicas Zr-MCM-41 were prepared by two different methods and characterized by XRD, TEM, nitrogen adsorption and EXAFS. In one method, tetraethoxysilane (TEOS) and zirconium tetra-n-propoxide (ZTNP) were mixed and TEOS and ZTNP were hydrolyzed and condensed in aqueous cetyltrimetylammonium bromide solution. EXAFS analysis revealed that zirconium species in Zr-MCM-41 prepared by this method aggregated each other and formed the bonds of Zr-O-Zr. This catalyst had a low catalytic activity for the peroxidative bromination of phenol red. In the other method, ZrCl4 and pure silica MCM-41 were used for impregnation. Zirconium species in this Zr-MCM-41 were highly dispersed as shown in the result of EXAFS analysis. This catalyst exhibited a high catalytic activity for the peroxidative bromination of phenol red. Zirconium species aggregated each other by calcination at 573 K, which caused reduction of catalytic activity.

XAFS Study on the Local Structure of Zirconium Containing Mesoporous Silicas, ZrMCM41 andTheir Catalytic Properties