Analysis of Structural Transformations during the Synthesis of a MoVTeNb Mixed Oxide Catalyst

This work presents a detailed investigation of the preparation routine for the multi-metal oxide Mo1V0.30Te0.23Nb0.125Ox used as catalyst for the selective oxidation of propane to acrylic acid. In-situ Raman spectroscopy on the initial aqueous polyoxometalate solution prepared from ammonium heptamolybdate, ammonium metavanadate and hexaoxotelluric acid reveals the coexistence of Anderson-type anions [TeM6O24]n-, M=Mo, V; n≥6, and protonated decavanadate species [HxV10O28](6-x)-. Raman analysis showed that the monomeric motif of the Anderson-type tellurate is preserved after addition of the Nb precursor and the subsequent spray-drying process. Calcination of the X-ray amorphous spray-dried material in air at 548 K seems to be the essential step, leading to a re-arrangement of the tellurate building blocks, generating nanocrystalline precursors of the phases finally established during treatment in helium at 873 K