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Ana Iglesias-Juez Gian Luca Chiarello Gregory S. Patience M. Olga Guerrero-Prez 《加拿大化工杂志》2022,100(1):3-22
Although X-ray absorption spectroscopy (XAS) was conceived in the early 20th century, it took 60 years after the advent of synchrotrons for researchers to exploit its tremendous potential. Counterintuitively, researchers are now developing bench type polychromatic X-ray sources that are less brilliant to measure catalyst stability and work with toxic substances. XAS measures the absorption spectra of electrons that X-rays eject from the tightly bound core electrons to the continuum. The spectrum from 10 to 150 eV (kinetic energy of the photoelectrons) above the chemical potential—binding energy of core electrons—identifies oxidation state and band occupancy (X-ray absorption near edge structure, XANES), while higher energies in the spectrum relate to local atomic structure like coordination number and distance, Debye-Waller factor, and inner potential correction (extended X-ray absorption fine structure, EXAFS). Combining XAS with complementary spectroscopic techniques like Raman, Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), and electron paramagnetic resonance (EPR) elucidates the nature of the chemical bonds at the catalyst surface to better understand reaction mechanisms and intermediates. Because synchrotrons continue to be the light source of choice for most researchers, the number of articles Web of Science indexes per year has grown from 1000 in 1991 to 1700 in 2020. Material scientists and physical chemists publish an order of magnitude articles more than chemical engineers. Based on a bibliometric analysis, the research comprises five clusters centred around: electronic and optical properties, oxidation and hydrogenation catalysis, complementary analytical techniques like FTIR, nanoparticles and electrocatalysis, and iron, metals, and complexes. 相似文献
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A cerium‐doped FePO4 catalyst dehydrates glycerol to acrolein in the gas phase but carbon accumulation reduces the reaction rate with time. Reaction rates may be maintained for longer times by co‐feeding low concentrations of oxygen together with the glycerol, but the acrolein yield drops proportionally to the oxygen concentration. The catalyst is easily regenerated by air and the reaction rate is proportional to both the oxygen concentration and quantity of carbon. The carbonaceous deposits may be due to both glycerol and acrolein: when either is fed to the catalyst, the CO2/CO ratio is close to 1; during the regeneration step, the CO2/CO ratio is near 4. A kinetic model of first order in both oxygen concentration and adsorbed sites characterizes the transient data very well. 相似文献
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Martin G. Bakker Benjamin Fowler Michael K. Bowman Gregory S. Patience 《加拿大化工杂志》2020,98(8):1668-1681
Electron paramagnetic resonance (EPR) spectroscopy, also known as electron spin resonance spectroscopy (ESR), utilizes absorption of microwave radiation by unpaired electrons in a magnetic field. The interaction between the unpaired electron(s) and nearby magnetic nuclei helps identify paramagnetic species and can provide information about the motion of the molecule and the local polarity, pH, viscosity, concentration, and accessibility to other paramagnetic species. This mini-review discusses the fundamental underpinnings of EPR needed to correctly interpret EPR spectra. We describe various types of EPR spectra encountered by chemical engineers, and use application examples drawn from the chemical engineering literature to illustrate the information available from the technique. Few chemical engineering departments or even chemistry departments have EPR instruments, which contributes to the significant barrier that prevents this being adopted as a routine measurement technique. However, in 2016 and 2017, Web of Science indexed 7000 articles that applied EPR spectroscopy. A bibliometric map categorized the keywords in four categories based on co-occurrences: magnetic properties, films, and luminescence; crystal structure, complexes, and ligands; nanoparticles, oxidation, and degradation; and, systems, radicals, and H2 O2 . 相似文献
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Raquel Ramos M. Pilar Pina Miguel Menndez Jesús Santamaría Gregory S. Patience 《加拿大化工杂志》2001,79(6):891-901
The reaction kinetics of the oxidative dehydrogenation of propane to propene over a V/MgO catalyst were studied. Both propane and propene oxidation kinetics were measured independently to quantify the rates of the parallel and consecutive reactions to propene and carbon oxides. Specific experiments to evaluate reaction products effects showed that water inhibited reaction rates but co‐feeding CO2 or propene had no measurable effect on selectivity or conversion. Kinetic data generated under integral reactor conditions and over an inert membrane reactor have also been used to estimate the kinetic parameters. Selectivity decreased as the oxygen partial pressure increased; however, propene yield was relatively insensitive to oxygen concentration. A dual site Mars‐van Krevelen model characterizes the reaction kinetics well. The role of lattice oxygen was established by alternating pulses of propane and oxygen. This redox model is able to predict the experimental tendencies observed in the three types of reactor studied. 相似文献
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