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A polyoxometalate–zirconia (POM/ZrO₂) nanocomposite was prepared through entrapment of H₃PW₁₂O₄₀ polyoxometalate into zirconia matrix by sol–gel technique involving the hydrolysis of zirconium (IV) n-butoxide, Zr(n-OBu)₄, as the ZrO₂ source. The catalyst was characterized by using XRD, FT-IR, SEM, TEM and surface area measurement and used as an efficient heterogeneous photocatalyst for aerobic oxidation of alcohols. Various primary and secondary benzylic alcohols were oxidized into the corresponding aldehydes and ketones in high yields under O₂ atmosphere in the presence of photoexcited POM/ZrO₂ nanocomposite. Also, nonactivated aliphatic alcohols were oxidized in good yields albeit after longer reaction times in comparison with benzylic alcohols, so that the selective oxidation of a benzylic OH group in the presence of a non-benzylic OH group could be achieved by the appropriate …