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Polyoxometalates (POM) supported on zirconia, H(3)PW(12)O(40)/ZrO2, were prepared by incorporating polyphosphotungstate into a zirconia matrix via sol-gel technique that involving the hydrolysis of zirconium (IV) n-butoxide, Zr (n-OBu)(4), as the ZrO(2) source. This insoluble and readily separable catalyst was characterized by using XRD, FT-IR, SEM, and UV diffuse reflectance spectroscopy (UV-DRS), indicating that the polyphosphotungstate was chemically attached to the zirconia supports, and primary Keggin structure remained intact. The photocatalytic and sonocatalytic activity of the supported polyphosphotungstate was tested via degradation of different dyes in aqueous solutions. The POM-ZrO(2) nanocomposite showed higher photocatalytic and sonocatalytic activity than pure polyoxometalate or pure ZrO(2).