Facultad Regional Córdoba
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Item Síntesis directa de CMK-3 modificada con Ti, como soporte de Ir aplicado a reacciones de hidrodenitrogenacion.(Univesidsad Tecnológica Nacional., 2018) Ledesma, Brenda Cecilia; Juárez, Juliana María; Beltramone , Andrea Raquel; Juárez, Juliana MaríaEn el presente trabajo se sintetizó Ti-CMK-3 mediante un nuevo método de síntesis, en el cual se evita la utilización de un molde, con el fin de reducir el tiempo, el consumo de energía y por ende el costo. La caracterización estructural y superficial del catalizador se realizó mediante adsorción de N2, XRD, UV-Vis DRS, espectroscopía Raman y TEM. Los resultados de la caracterización indicaron que las propiedades texturales y estructurales del material sintetizado son comparables con las propiedades del material preparado por el método tradicional. El catalizador Ir-Ti-CMK-3 obtenido fue activo y selectivo para la reacción de hidrodenitrogenación (HDN) del indol. La principal ventaja del presente estudio es la reducción de tiempo y costo de la síntesis, simultáneamente con la aplicabilidad en las reacciones de Hidrotratamiento (HDT)Item Direct Synthesis of ordered mesoporous carbon as support of Ir-Catalyst and its application in hydrodenitrogenation of indole.(Univesidsad Tecnológica Nacional., 2018) Ledesma, Brenda Cecilia; Juárez , Juliana María; Beltramone, Andrea Raquel; Juárez , Juliana MaríaAn ordered mesoporous carbon (OMC) modified with titania was prepared using a novel and shorter synthesis method. OMC was successfully synthesized by the carbonization of the silica/TEOT/triblock copolymer/sucrose composite in the presence of sulfuric acid. This novel material was modified with the incorporation of nanoparticles of Iridium. Structural and textural characterization of the catalyst was performed by means of N2 adsorption, XRD, UV–Vis–DRS, Raman spectroscopy, XPS, TEM and H2 Chemisorption. The characterization results indicated that the textural and structural properties of the support synthesized by the short time method are comparable with the properties of the support prepared by the hard template method. Ir-Ti-OMC catalyst obtained by short time synthesis was active and selective in the hydrogenation of indole. Main advantage of the present study is the reduction of time and cost in the synthesis of the new material and the applicability for HDT reactions.Item Sulfur elimination by ODSwith titanium-modified SBA-16.(Univesidsad Tecnológica Nacional., 2015) Rivoira , Lorena Paola; Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Martínez , María Laura; Anunziata , Oscar Alfredo; Beltramone , Andrea Raquel; Anunziata , Oscar Alfredo; Martínez , María Laura; Ledesma, Brenda; Vallés , Verónica AlejandraNanostructured carbon CMK-3 and mesoporous silica SBA-15 modified with Fe by using different sources of Fe, were used in the oxidative desulfurization (ODS) of dibenzothiophene (DBT) as a model sulfur compound. Fe-CMK-3 and Fe-SBA-15 were prepared by wetness impregnation using FeCl3.6H2O and FeNO3.9H2O as different sources of Fe. A solution of FeCl3.6H2O/ FeNO3.9H2O in ethanol was mixed with the corresponding material solution (CMK-3 or SBA-15) at room temperature. The solution was placed in a rotary evaporator to remove excess of ethanol at about 333 K and 60 rpm. Afterwards, the sample was dried at 373 K for 18 h and was thermally treated in a dynamic inert (N2) atmosphere. The percentage of Fe has been 2 wt.% with respect to carbon in the final FeCl3-CMK-3 and FeNO3-CMK-3 material. Four samples modified with Fe have been prepared and were characterized by XRD, FTIR, XPS, BET, TEM and SEM. These studies indicated that it was possible to obtain a CMK-3 replica successfully from SBA-15, using sucrose as a carbon precursor. Wide angle XRD pattern of the sample modified with FeCl3.6H2O implies the formation of the magnetite phase in the silica channels. The nanomaterial area is significantly smaller with the incorporation of the metal, SBA-15 and CMK-3`s characteristic structure is maintained after the metal is within the host, in agreement with the XRD studies. The catalytic activity was improved when the nanoporous materials were modified with Fe. The nanoporous carbon modified with FeCl3.6H2O was the most active catalyst for ODS of DBT, using hydrogen peroxide (H2O2) as oxidant and acetonitrile as solvent. 100% of DBT elimination was attained at a short time in mild conditions.Item CMK-3 modificada con titanio obtenida mediante un novedoso y rápido método de síntesis aplicada en la desulfuración oxidativa de compuestos organosulfurados.(Univesidsad Tecnológica Nacional., 2018) Rivoira , Lorena Paola; Ledesma, Brenda Cecilia; Juárez , Juliana María; Beltramone , Andrea Raquel; Juárez , Juliana María; Ledesma, BrendaEl nanomoldelado de materiales ha sido el único método para crear materiales mesoporosos de carbono, utilizando plantillas inorgánicas (Ezzeddine et al., 2016). Involucra una última etapa donde se elimina el agente plantilla, lo cual lo hace complicado, largo y de elevado costo. Recientemente Ledesma et al. (2017) demostraron la posibilidad de un método de síntesis más corto para obtener CMK-3 modificada con Ti incorporando las especies de Ti directamente en la estructura del carbón mesoporoso utilizando Ti-SBA-15 como agente plantilla. En la reacción de ODS ocurre la oxidación de aquellos compuestos de S más refractarios en la HDS, utilizando de un agente oxidante en presencia de un catalizador (Subhan et al., 2012). Es necesario agregar un solvente polar al sistema, capaz de extraer las moléculas de S desde la fase diesel para que pueda estar en contacto con el agente oxidante (H2O2, polar) y el catalizador. En el presente trabajo se evalúa la actividad en la ODS de carbón mesoporoso CMK-3 modificado con Ti, sintetizado mediante un novedoso método más corto.Item Experimental Desing Optimization of the tetralin Hydrogenation over Ir-Pt-SBA-15.(Univesidsad Tecnológica Nacional, 2016) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma, BrendaExperiment design-response surface methodology (RSM) is used in this work to model and optimize two responses in the hydrogenation of tetralin to decalin using bimetallic Ir–Pt-SBA-15 catalyst. In this study, we analyze the influence of the nature of the catalyst (metal molar fraction and metal loading), the catalyst/substrate ratio and the temperature of the reaction as factors for the design. The responses analyzed were conversion at 3 h and at 5 h of reaction time. The response surfaces were obtained with the Box–Behnken design, finding the best combination between the reaction parameters that allowed optimizing the process. By applying the statistic methodology, the higher levels of the two objective functions were obtained employing the catalyst with 1 wt.% of iridium and 0.7–0.8 wt.% of platinum; the optimal ratio between mass of catalyst and mole of tetralin was 17–19 g/mol and temperature between 200 and 220 ◦C.Item Hidrogenación de tetralin sobre Ir-Pt-SBA-15. Parte 2: Optimización por Diseño de Experimentos.(Univesidsad Tecnológica Nacional, 2015) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone , Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma, BrendaLa Metodología Diseño de Experimentos - Superficie de Respuesta – se utiliza en este trabajo para modelar y optimizar 2 respuestas en la reacción de hidrogenación de tetralin a decalin usando un catalizador bimetálico Ir-Pt-SBA-15. En este estudio se analizó la influencia de la naturaleza del catalizador, la relación catalizador/sustrato y la temperatura de reacción como factores del diseño. Las respuestas analizadas fueron conversión a 3 y 5 horas Las Superficies de Respuesta fueron obtenidas mediante un diseño Box-Behnken a fin de encontrar la mejor combinación de los distintos parámetros para optimizar el proceso. La metodología estadística aplicada indica que las conversiones más altas de ambas respuestas, a 3 y 5 horas, se obtienen trabajando en el siguiente rango: Catalizador: 1% Ir y 0.7-0.9 %(p/p) Pt; Relación: 17-19 g cat/ mol TL y Temperatura: 200-220°C.Item Hidrogenación de tetralin sobre Ir-Pt-SBA-15. Parte 1: Síntesis, caracterizacíon y actividad catalítica.(Univesidsad Tecnológica Nacional, 2015) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone , Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena PaolaSe estudia aquí la hidrogenación de tetralin a decalin utilizando un catalizador bimetálico Ir-Pt SBA-15. En esta Parte se describe la síntesis de los catalizadores, la preparación de la matriz de SBA 15 y el método de co-impregnacion mediante el cual se incorporaron los metales en diferentes proporciones y carga total metalica. Los catalizadores fueron caracterizados por XRD, TEM, análisis fisicoquimicos, XPS, SEM y EDX. En la Parte 2 de este trabajo se analizará la influencia de la naturaleza del catalizador, la relación catalizador sustrato y la temperatura de reacción como factores de un Diseño de Experimentos para optimizar el proceso.Item Síntesis y caracterización de un catalizador soportado iridio/platino-SBA-15 para su aplicación en la Hidrogenación de Tetralin.(Univesidsad Tecnológica Nacional, 2014) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira , Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Rivoira , Lorena Paola; Ledesma, BrendaIn this paper the effect of the dispersion of noble metals Ir and Pt and interaction with the SBA-15 support was studied by relating them to the catalytic activity of the catalyst in the hydrogenation reaction of Tetralin using a Parr reactor at 250°C and 15 atm. With this objective Ir/Pt-SBA-15 modified catalysts were synthesized with different % of Ir and Pt. The mesostructure of SBA-15 support gives a relatively high thermal stability and proper pore diameter can converts large molecules such as those present in the liquid fuels. The support was prepared by the sol-gel method. The catalytic site was obtained using incipient co impregnation method. The material was characterized by X-ray diffraction (XRD) and TEM). The metal dispersion was calculated by H2 chemisorption and TEM. Iridium / Platinum particles (d = 2,0-4,0 nm) homogeneously dispersed were obtained with a dispersion of more than 60%.Item Tetralin hydrogenation over Ir-Pt/SBA-15. optimization by experimental desing.(Univesidsad Tecnológica Nacional, 2024) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira, Lorena Paola; Cussa , jorgelina; Anunziata , Oscar Alfredo; Beltramone , Andrea Raquel; Anunziata , Oscar Alfredo; Cussa , jorgelina; Ledesma, BrendaBimetallic catalysts have received considerable attention for hydrotreating (HDT) because they show high activity. The features of the catalysts here studied are going to be correlated with their catalytic performance in the hydrogenation of tetralin at mild conditions. The final goal is to find the optimal proportion of each metal in order to be more active and the best reaction conditions (temperature and amount of catalyst). The statistical experiments design is the process of planning an experiment to obtain appropriate data that can be analyzed by statistical methods, to produce concrete and valid conclusions. One of the main advantages in the response curve is to visualize the response for all levels of the experimental factors Experiment design response surface methodology (RSM) is used in this work to model and to optimize the process. Platinum and Iridium nanoparticles were incorporated into SBA-15 support by the wet co impregnation method. Ir content was set as 1wt. % and Pt was varied from 0 to 1wt. %. The catalysts were characterized by XRD, BET, XPS, TEM, ICP and TPR. XRD profiles are characteristic of the two-dimensional p6mm hexagonal mesostructure with d100 spacing of 10.16 nm; where the d100 spacing upon Ir and Pt incorporation were quite similar to pristine SBA-15. The TEM images and XPS demonstrate that the metal particles were mainly present inside the porous and XPS and TPR corroborated the reduced state of the metals. The catalytic activity was measured in a 4563Parr reactor at 15 atm of hydrogen and 360 rpm. Feed consisted in 50 mL of tetralin in Dodecane, the amount of tetralin is set according to the ratio of catalyst mass/mass reagent corresponding to each reaction. The application of this methodology allows a better understanding of the influence of the different factors: content of metal on catalyst (A), relationship: mass of catalyst/reagent mass (B) and reaction temperature (C), on two responses: conversion at 3 h and at 5 h of reaction time. These factors were carefully selected taking account the influence of the parameters in the reaction. The design was analyzed by Statgraphics and Statistica Soft. We found that, the variable Catalyst has the best influence over the Conversion at the 95.0% confidence level, according to the Pareto.Item Hidrogenación de tetralin utilizando un catalizador bifuncional de iridio/platino-SBA-15.(Univesidsad Tecnológica Nacional, 2014) Vallés , Verónica Alejandra; Ledesma, Brenda Cecilia; Rivoira, Lorena Paola; Cussa , jorgelina; Martínez , María Laura; Anunziata , Oscar Alfredo; Beltramone, Andrea Raquel; Anunziata , Oscar Alfredo; Martínez , María; Cussa , jorgelina; Ledesma, BrendaLos catalizadores bimetálicos de Pt–Pd han recibido considerable atención debido a que demuestran tener una alta actividad en una amplia variedad de aplicaciones catalíticas (1). Con alta actividad, selectividad y estabilidad, comparada con catalizadores monometálicos de Pt y Pd. Por ejemplo, catalizadores bimetálicos Pt-Pd muestran tener mayor resistencia frente a envenenamientos en comparación con catalizadores de Pt (2-4). Las características estudiadas del catalizador serán correlacionadas con su performance catalítica en la hidrogenación del tetralin. El objetivo final es encontrar la proporción óptima de cada uno de los metales de forma de lograr la mayor actividad en dicho proceso.
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