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Producción sustentable de hidrógeno empleando metales nobles soportados sobre materiales nanoestructurados basados en CeO_2. / Sustainable hydrogen production using noble metals supported on nanostructured CeO2-based materials.

Carbajal Ramos, Inés A. (2014) Producción sustentable de hidrógeno empleando metales nobles soportados sobre materiales nanoestructurados basados en CeO_2. / Sustainable hydrogen production using noble metals supported on nanostructured CeO2-based materials. Tesis Doctoral en Ciencias de la Ingeniería, Universidad Nacional de Cuyo, Instituto Balseiro.

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La presente Tesis de Doctorado en Ciencias de la Ingeniería comprende la síntesis de metales soportados sobre materiales basados en ceria y la caracterización estructural, microestructural, textural y química de los mismos. Estos materiales fueron usados como catalizadores de la reacción de reformado de etanol con vapor de agua para la producción de hidrógeno. Se sintetizaron dos tipos de soportes basados en ceria: en uno, el CeO_2 se depositó por impregnación sobre ZrO_2 estabilizado con ytria (YSZ) de origen comercial (CeO_2(10%p/p)/YSZ) y en el otro, se preparó una solución sólida de CeO_2-ZrO_2 (Ce_0,8Zr_0,2O_2) empleando dos métodos de síntesis diferentes: uno clásico, conocido como co-precipitación (PI) y otro novedoso, que involucra el procesamiento mecanoquímico (HW) y consistió en preparar la solución sólida Ce_0,8Zr_0,2O_2 a partir de la molienda mecánica de los cloruros de Ce y Zr, en presencia de NaOH. Sobre ambos soportes se dispersaron las fases metálicas activas por el método de impregnación. Sobre CeO_2(10%p/p)/YSZ) se depositaron Ru 2 % p/p (Ru/CeO_2/YSZ), Pd 2 % p/p (Pd/ CeO_2/YSZ) y Ag 2 % p/p (Ag/ CeO_2/YSZ). Luego fueron calcinados por 5 h a 400 °C. Sobre Ce_0,8Zr_0,2O_2 (PI y HW) se depositaron los metales Ru 2 % p/p (Ru2PI y Ru2HW), Pd 2 % p/p (Pd2PI y Pd2HW), Ni 2 % p/p (Ni2PI y Ni2HW) y Ni 8 % p/p ( (Ni8PI y Ni8HW). Luego fueron calcinados por 5 h a 600 °C. Todos estos catalizadores fueron evaluados en la reacción de reformado de etanol con vapor de agua para la producción de hidrógeno. Dentro de la serie M/CeO_2/YSZ (M = Ru, Pd, Ag) los sistemas basados en Ru y Pd mostraron actividades promisorias, mientras que el catalizador con Ag presentó un pobre desempeño. Se observaron pequeñas cantidades de coque en ambos catalizadores: sobre Pd/CeO_2/YSZ conduce a la oclusión de las nanopartículas metálicas, dando como resultado una progresiva y drástica desactivación del catalizador; en el caso del catalizador Ru/CeO_2/YSZ se observa una cantidad menor de carbono en forma de filamentos grafíticos que produce una mayor accesibilidad al Ru. Dentro de las series MZPI y MZHW (M = Ru, Pd, Ni; Z = 2 y 8), los sistemas basados en Ru (2 %) y Ni (8 %) mostraron actividades promisorias, mientras que los catalizadores con Pd presentaron muy bajos rendimientos. En condiciones moderadas y leves, el desempeño del catalizador estuvo gobernado por la naturaleza de la fase metálica, la del soporte y por la interacción entre ambos. En cambio, en condiciones de reformado severas, los metales sobre el soporte PI presentaron mejor desempeño que sobre HW. Los catalizadores basados en Ni condujeron a la formación de grandes cantidades de coque, el cual pudo ser removido a temperaturas moderadas y por lo tanto es factible su regeneración. En el caso del catalizador de Ru, no se observó deposición de coque y presentó la más alta selectividad a hidrógeno. Finalmente, es destacable el excelente desempeño catalítico observado para el catalizador de Ru2PI. La adecuada combinación de las propiedades del soporte y de la interacción con la fase metálica, posibilita una alta dispersión del metal Ru y por ende una alta selectividad a hidrógeno, sin depósitos de coque y con una buena relación CO/CO_2. Este constituye un resultado original y hasta la fecha se desconoce el mecanismo de reacción, por lo que este aspecto será abordado en futuras investigaciones.

Resumen en inglés

This Ph.D Thesis in Engineering Science includes the synthesis of metals supported on ceria-based materials and their structural, microstructural, textural and chemical characterization. These materials were used as catalysts in the steamreforming of ethanol for hydrogen production. Two types of ceria-based supports Were synthesized: added by impregnation on comercial ytria-stabilized zirconia (CeO_2(10%p/p)/YSZ) and solid solution of CeO_2- ZrO_2 (Ce_0.8Zr_0.2O_2). The latter, making use of two different synthesis methods: the classic method known as co-precipitation (PI), and an innovative one which involves the mecanochemical proccesing (HW) and consists in preparing the Ce_0.8Zr_0.2O_2 solid solution from mechanical milling of CeCl_3 and ZrCl_4 in presence of NaOH. The metallic active phases were added on both supports by the impregnation method. Ru 2 % p/p (Ru/CeO_2/YSZ), Pd 2 % p/p (Pd/ CeO_2/YSZ) and Ag 2 % p/p (Ag/ CeO_2/YSZ) were supported on CeO_2(10 %p/p)/YSZ), then calcined for 5 h at 400 ºC. Ru 2 % p/p (Ru2PI and Ru2HW), Pd 2 % p/p (Pd2PI and Pd2HW), Ni 2 % p/p (Ni2PI and Ni2HW) and Ni 8 % p/p (Ni8PI and Ni8HW) were supported on Ce_0,8Zr_0,2O_2 (PI and HW) ), then calcined for 5 h at 600 ºC. All these catalysts were evaluated in the steam-reforming of ethanol for hydrogen production. Ru and Pd-based systems showed promising activities within the M/CeO_2/YSZ (M = Ru, Pd, Ag) series, while Ag catalysts showed a low performance. Small amounts of coke were observed on both catalysts, on Pd/CeO_2/YSZ it leads to the occlusion of the metallic nanoparticles, resulting in a progressive and dramatic catalyst deactivation, while a smaller amount of graphite filament-shaped carbon is observed on Ru/CeO_2/YSZ, resulting in a greater accessibility to Ru. Ru(2%) and Ni(8%) showed promising activities within the MZPI and MZHW (M = Ru, Pd, Ni; Z = 2 and 8) series, while Pd catalysts showed a poor performances. The catalyst’s performance, under moderate and mild conditions is governed by the metallic phase’s nature, the support phase’s nature and their mutual interaction. On the other hand, under severe reforming conditions the metals on the PI support show a better performance than HW. Ni-based catalysts lead to a great coke production which can be removed at moderate temperatures, and therefore are feasible to be regenerated. For Ru catalysts, carbon-deposition is not observed and this catalyst shows the highest hydrogen selectivity. Finally it must be pointed out the excellent catalytic performance showed by the Ru2PI catalyst. The adequate combination of the support’s properties and the interaction with the metallic phase enables a high dispersion of Ru and therefore high hydrogen selectivity without carbon deposition and with a good CO/CO_2 ratio. This is an original result and up to now the reaction mechanism is unknown, for which this aspect will be addressed in future research.

Tipo de objeto:Tesis (Tesis Doctoral en Ciencias de la Ingeniería)
Palabras Clave:Hydrogen; Hidrógeno; Catalysis; Catálisis; Ethanol; Etanol; Nanostructures; Nanoestructuras; [Ceria]
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Materias:Química > Química analítica
Física > Física de materiales
Química > Química física
Divisiones:Gcia. de área de Aplicaciones de la tecnología nuclear > Gcia. de Investigación aplicada > Fisicoquímica de materiales
Código ID:484
Depositado Por:Marisa G. Velazco Aldao
Depositado En:17 Abr 2015 15:55
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