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Gas phase dehydration of glycerol to acrolein over WO₃-based catalysts prepared by non-hydrolytic sol-gel synthesis.

ABSTRACT: Solid acid catalysts based on WO₃-SiO₂ and WO₃-ZrO₂-SiO₂ were prepared by one-pot non-hydrolytic sol-gel method and tested in the gas phase glycerol dehydration to acrolein. Their structural and textural characteristics were determined by X-ray diffraction (XRD), N₂ adsorption, X-ray energy dispersive spectroscopy (XEDS), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). Their acid characteristics were studied by both temperature programmed desorption of ammonia (NH₃-TPD) and FTIR of adsorbed pyridine. Under our operating conditions, all the catalysts were active and selective in the transformation of glycerol to acrolein, which was always the main reaction product. The high selectivity to acrolein is achieved on catalysts presenting a higher proportion of Brønsted acid sites. In addition, the role of oxygen in the feed on catalytic performance of these catalysts is also discussed.

SUBMITTER: Nadji L

PROVIDER: S-EPMC9079827 | biostudies-literature | 2018 Apr

REPOSITORIES: biostudies-literature

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Gas phase dehydration of glycerol to acrolein over WO3-based catalysts prepared by non-hydrolytic sol-gel synthesis.

Nadji L L Massó A A Delgado D D Issaadi R R Rodriguez-Aguado E E Rodriguez-Castellón E E Nieto J M López JML

RSC advances 20180410 24

Solid acid catalysts based on WO3-SiO2 and WO3-ZrO2-SiO2 were prepared by one-pot non-hydrolytic sol-gel method and tested in the gas phase glycerol dehydration to acrolein. Their structural and textural characteristics were determined by X-ray diffraction (XRD), N2 adsorption, X-ray energy dispersive spectroscopy (XEDS), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS). ...[more]

PMID: 35542536

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Project description:Titanium dioxide (TiO2) in the form of thin films has attracted enormous attention for photocatalysis. It combines the fundamental properties of TiO2 as a large bandgap semiconductor with the advantage of thin films, making it competitive with TiO2 powders for recycling and maintenance in photocatalytic applications. There are many aspects affecting the photocatalytic performance of thin film structures, such as the nanocrystalline size, surface morphology, and phase composition. However, the quantification of each influencing aspect needs to be better studied and correlated. Here, we prepared a series of TiO2 thin films using a sol-gel process and spin-coated on p-type, (100)-oriented silicon substrates with a native oxide layer. The as-deposited TiO2 thin films were then annealed at different temperatures from 400 °C to 800 °C for 3 h in an ambient atmosphere. This sample synthesis provided systemic parameter variation regarding the aspects mentioned above. To characterize thin films, several techniques were used. Spectroscopic ellipsometry (SE) was employed for the investigation of the film thickness and the optical properties. The results revealed that an increasing annealing temperature reduced the film thickness with an increase in the refractive index. Atomic force microscopy (AFM) was utilized to examine the surface morphology, revealing an increased surface roughness and grain sizes. X-ray diffractometry (XRD) and UV-Raman spectroscopy were used to study the phase composition and crystallite size. The annealing process initially led to the formation of pure anatase, followed by a transformation from anatase to rutile as the annealing temperature increased. An overall enhancement in crystallinity was also observed. The photocatalytic properties of the thin films were tested using the photocatalytic decomposition of acetone gas in a home-built solid (photocatalyst)-gas (reactant) reactor. The composition of the gas mixture in the reaction chamber was monitored using in situ Fourier transform infrared spectroscopy. Finally, all of the structural and spectroscopic characteristics of the TiO2 thin films were quantified and correlated with their photocatalytic properties using a correlation matrix. This provided a good overview of which film properties affect the photocatalytic efficiency the most.

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Gas phase dehydration of glycerol to acrolein over WO₃-based catalysts prepared by non-hydrolytic sol-gel synthesis.

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Gas phase dehydration of glycerol to acrolein over WO<sub>3</sub>-based catalysts prepared by non-hydrolytic sol-gel synthesis.

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