Barium molybdate and Barium tungstate are important materials due their photoluminescent properties and they also have catalysis and photocatalysis applications. In this work, powders of these compounds were prepared by microwave-assisted hydrothermal (MAH) method and polymeric precursor method (PPM) and their structural and optical properties were studied. Furthermore, these materials were employed as solid catalysts towards gas phase toluene oxidation reactions. X-ray diffraction confirms the purity of materials at both preparation methods and reveals a preferential growth when the powders are prepared by MAH due polymeric agents and processing using microwave, which was confirmed by Field emission scanning electron microscopy. Photoluminesce emission was attributed to the charge-transfer transitions within the [WO 4 ] 2and [MoO 4 ] 2complexes. The H 2 Temperature-Programmed Reduction (H 2 -TPR), O 2 -chemisorption and extended X-ray absorption fine structure (EXAFS) results indicated that BaWO 4 samples, compared with BaMoO 4 samples, have higher oxygen mobility and oxygen vacancies that appear as key factors for the achievement of better catalytic performances.
Calcium tungstate (CaWO 4) crystals were prepared by microwave-assisted hydrothermal (MAH) and polymeric precursor methods (PPM). These crystals were structurally characterized by X-ray diffraction (XRD), N 2 adsorption, X-ray absorption near edge spectroscopy (XANES) and extended X-ray absorption fine structure (EXAFS) measurements. The morphology and size of these crystals were observed by field emission scanning electron microscopy (FE-SEM). Their optical properties were investigated by ultraviolet visible (UV-Vis) absorption and photoluminescence (PL) measurements. Moreover, these materials were employed as catalysts towards gas phase toluene oxidation reaction. XRD indicates the purity of materials for both preparation methods and MAH process produced crystalline powders synthesized at lower temperatures and shorter processing time compared to the ones prepared by PPM. FE-SEM images showed particles with rounded morphology and particles in clusters dumbbellslike shaped. PL spectra exhibit a broad band covering the visible electromagnetic spectrum in the range of 360 to 750 nm. XANES and EXAFS results show that preparation method does not introduce high disorders into the structure, however the H 2-TPR results indicated that the catalyst reducibility is affected by the preparation method of the samples.
The oxidation of sulfides to sulfoxides and sulfones provides valuable sulfur-containing chemical compounds that are used in the pharmaceutical agrochemical industry. Although some tungsten catalytic systems have been applied to sulfide oxidation, the most desirable heterogeneous catalytic protocols have not been described. The copper, nickel and zinc tungstates powders obtained by the polymeric precursor method and the evaluation of their catalytic activity in thioanisole oxidation were investigated. Thioanisole was oxidized by hydrogen peroxide to sulfoxides and sulfones and the presence of catalyst accelerates the conversion. Of the three catalysts, copper tungstate was the most efficient in the conversion process followed by nickel tungstate and finally zinc tungstate. The copper tungstate has higher hydrogen consumption, indicating a higher oxygen content on the surface and the ability to increase surface mobility, which increases the conversion and selectivity of the process. The addition of 0.1 mL of hydrogen peroxide enhanced the conversion and increased the amount of sulfone produced. The ideal reaction time was 12 hours and the optimum temperature was 75 °C.
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