The catalytic properties of nCrOx/Al2O3 nanoparticles (n = 4.8 ± 0.05 wt %) tested in the isobutane dehydrogenation reaction which were obtained by laser synthesis in various gases are studied in detail for the first time. Laser synthesis of 4.8% CrOx/Al2O3 nanopowders was carried out by the vaporization of 5.0% Cr : α-Al2O3 ceramic targets using cw CO2 laser irradiation in an inert, oxidizing and reducing gaseous environment in a vaporization chamber: in an Ar medium; Ar with addition of O2, H2 and CH4 at concentrations of 20, 30, and 13 vol. %, respectively. The role of the gas medium during the synthesis of 4.8% CrOx/Al2O3 nanopowders in their catalytic properties (activity, selectivity, conversion, and stability in the reaction) was determined. A comprehensive study of the physicochemical properties of the obtained nanocatalysts was carried out using XRD, TEM, UV-Vis DRS, and Raman techniques. According to XRD data the phase composition is predominantly consists of γ-Al2O3 with the beginning of the transition to δ-Al2O3. According to the TEM results, the shape of nanoparticles is spherically symmetric with an average particle size dm = 15 nm. Using the UV-Vis DRS method, charge states of Crq+ (q = 3, 6) in different coordination (Cr6+(Td) and Cr3+(Oh)) and its different ratios depending on the gas atmosphere used in the process of laser vaporization were revealed in the obtained 4.8% CrOx/Al2O3 nanopowders. Nanosized 4.8% CrOx/Al2O3 catalyst prepared in an atmosphere (Ar + H2) demonstrated the highest values of isobutane conversion (39%) and isobutylene selectivity (90.7%); the lowest corresponding values of conversion (18.8%) and selectivity (85.6%) were typical for the sample obtained in the atmosphere (Ar + CH4). Thus, the most active and selective in the isobutane dehydrogenation reaction was the 4.8% CrOx/Al2O3 nanocatalyst synthesized in the (Ar + H2) medium, and the presence of methane during vaporization led to the initial surface carbonization, which prevents the access of reacting molecules to it.
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