Marco Daturi, José Rodríguez-Mirasol, M.O. Guerrero-Pérez, Tomás Cordero, Philippe Bazin, Juan José Ternero-Hidalgo, Raquel Portela, Miguel A. Bañares, Guillaume Clet, Universidad de Málaga [Málaga] = University of Málaga [Málaga], Instituto de Catálisis y Petroleoquímica (ICP), Consejo Superior de Investigaciones Científicas [Madrid] (CSIC), Laboratoire catalyse et spectrochimie (LCS), Centre National de la Recherche Scientifique (CNRS)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Normandie Université (NU)-Institut de Chimie du CNRS (INC)-Université de Caen Normandie (UNICAEN), Normandie Université (NU), Ministerio de Economía y Competitividad (España), Ministerio de Ciencia, Innovación y Universidades (España), Centre National de la Recherche Scientifique (France), Portela, Raquel [0000-0002-1882-4759], Instituto de Catalisis y Petroleoquimica (CSIC), Université de Madrid, Université de Caen Normandie (UNICAEN), Normandie Université (NU)-Normandie Université (NU)-École Nationale Supérieure d'Ingénieurs de Caen (ENSICAEN), Normandie Université (NU)-Centre National de la Recherche Scientifique (CNRS), and Portela, Raquel
Raman and transmission FTIR spectroscopic techniques have been coupled in a new homemade reactor-cell designed in a joint CSIC-LCS collaboration. The setup is easily adapted to any FTIR and fiber-coupled Raman spectrometers and gas analysis techniques. It allows for simultaneous operando FTIR and Raman spectroscopic measurement, which provide complementary characterization of adsorbed species, reaction intermediates, and structural properties of the catalyst. This system was validated with the study of vanadium-based catalysts during propane oxydehydrogenation (ODH). The combined use of both spectroscopies with gas analysis techniques to measure the activity contributes to the understanding of propane ODH and the identification of the role of different oxygen species bound to vanadium sites. For example, the simultaneous characterization of the catalyst under the same conditions by IR and Raman confirms that the V═O mode has the same frequency in both spectroscopies and that bridging oxygen sites (V - O - V, V - O - Zr) present higher activity than terminal V═O bonds. These results demonstrate the high potential of the new simultaneous transmission IR-Raman operando rig to correlate the activity and the structure of catalysts, thus assisting the rational design of catalytic processes., Authors acknowledge the FEDER-Region Basse-Normandie (France)-CNRS for a Chaire d’Excellence, which resulted in the implementation of the “IRRaman” rig and a research stay allowing for the performance of these investigations. This work was also supported by the Spanish Ministry of Economy and Competitiveness and FEDER (CTQ2012-36408, CTQ2015-68654-R, and CTM2017-82335-R). J.J.T.H. acknowledges the assistance of the Ministry of Economy and Competitiveness of Spain for the award of a FPI Grant (BES-2013-064425) and the award for performing his stay at ENSICAEN (EEBB-I-16-10749).