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.