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The influence of high content of MoO3 (32mol%) in V2O5–MoO3–P2O5 catalyst system supported on alumina, silica, HZSM-5 and modified clay was investigated for ammoxidation of 3-picoline. Unsupported VMPO catalyst and supported catalysts were prepared by incipient wet impregnation method keeping the mole ratio of V2O5–MoO3–P2O5 (1.00:3.27:0.14) constant. FT-IR spectra and X-ray diffractograms showed interaction among the active oxides and the support. The major phases identified were Mo4V6O25, Mo6V9O40 and MoV2O8. TG–DTA also showed the exothermic peaks indicating the formation of new compounds above 400°C. The physico-chemical properties of the catalysts were correlated with their activity and selectivity for ammoxidation of 3-picoline. The unsupported catalyst showed 96.0% selectivity whereas VMPO/HZSM-5 showed the highest selectivity (91.3%) amongst the supported catalysts. [Copyright &y& Elsevier]