VOHPO 4 AE 0.5H 2 O synthesized by VOPO 4 AE 2H 2 O and isobutanol was activated in a flow of propane/air mixture (1% propane in air) at 673 K for 36, 75 and 132 h. Three vanadyl pyrophosphate catalysts obtained were denoted as VPD36P, VPD75P and VPD132P. The crystallinity of all propane/air pretreated catalysts as shown in XRD increased with the duration of calcination. SEM micrographs showed the formation of more isolated platelets and more prominent rosebud-shape agglomerate as the pretreatment was longer. Four reduction peaks maxima at 752, 920, 1026 and 1140 were observed in the rate of hydrogen consumption for VPD36P. As the calcination duration increased to 75 h, the H 2 reduction peaks were shifted to lower temperatures at 750, 882, 1004 and 1140 K. When the calcination duration was further increased to 132 h, only three reduction peaks were observed at 752, 952 and 1142 K. Despite the progressively shifted of the major reduction peak maximum as the duration of calcination increased from 36 to 132 h, the lattice oxygen from VPD36P was found to be the most reactive. The catalytic performance for propane oxidation to acrylic acid (AA) showed that VPD36P gave the highest activity (9.6%) with 83.0% of selectivity to AA.
Vanadium phosphate catalysts were synthesized via VOPO42H2O and were calcined in two different hydrocarbon reaction environments, i.e.n-butane/air and propane/air. Both catalysts are denoted VPDB and VPDP, respectively. Both catalysts exhibited a good crystalline with characteristic peaks of pyrophosphate phase. However, the peaks for VPDP are shown to be more prominent than those of VPDB. BET surface area showed that VPDB gave higher surface area (23 m2 g1) compared to VPDP (18 m2 g1). The average V valence state for VPDP is 4.08 and the higher V valence state for VPDB is 4.26 due to higher amount of VV for VPDB. Furthermore 14.2% of VIII was found for VPDP but none for VPDB. SEM micrographs clearly revealed that the morphologies of both catalysts composed of plate-like crystallite that was arranged into the characteristic of rosette cluster. However, the catalyst calcined in n-butane/air environment (VPDB) resulted in an increment of the amount of plate-like crystal formed in the rosette rosebud agglomerates. TPR in H2 profiles of both catalysts gave two reduction peaks corresponding to two kinetically different oxygen species which were associated with VVand VIV phases, respectively. VPDB removed larger amount of active oxygen species linked to VIV phase which eventually caused a higher conversion rate in the selective oxidation of n-butane and propane to maleic anhydride and acrylic acid, respectively.
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