New highly active and selective nanostructured oxide catalysts. M. Olga Guerrero Pérez, Ricardo López-Medina Miguel A. Bañares
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1 New highly active and selective nanostructured oxide catalysts M. Olga Guerrero Pérez, Ricardo López-Medina Miguel A. Bañares Málaga, March 24th, 2008
2 What is a nanostructured catalysts? The catalytic active phase is nanoscaled on the surface of a support
3 Nanostructured catalysts active phase support bulk catalysts supported catalysts
4 Main advantages: Industrial point of view: Less expensive catalysts Academic point of view: Support can modulate the activity Better insight on the nature of the active phase
5 Characterization of the surface Reactant Product Reactant Product Usually Catalytic we obtain reaction information Nanostructured takes about place catalysts chemical on the surface structure of catalysts of the bulk
6 Reactant Product Reactant Product Support Coverage Additives Structure Activity-selectivity Activation / deactivation
7 Case 1: Sb-V-O catalytic materials for propane ammoxidation NH 3 +O 2 +C 3 H 8 CH 2 =CH-CN
8 Case 1: VSbO 4 on alumina Sb-V-O/Al 2 O 3 Sb+V < low coverage not active (surface vanadia) Guerrero-Pérez et al. (2002) VOx Al 2 O 3 SbOx Sb+V high coverage active (VSbO 4 phase) Grasselli et col. (1992) Guerrero-Pérez et al. (2002) Al 2 O 3 V-Sb-O VSbO 4 phase on alumina is not stable at low coverages Like the bulk system, VSbO 4 phase further forms during time-on-stream hydroxypyruvic acid mesoxalic acid
9 Case 1: Uncovering reaction mechanism by operando spectroscopy
10 Case 1: Uncovering reaction mechanism by operando spectroscopy Dominant phase, during ammoxidation: VSbO 4 + Sb 2 O Sb 2 O 3 Sb 2 O 4 during reoxidation: VOx + VSbO 4 + Sb 2 O VSbO 4 phases 5+ O V / \ O O O Ammoxidation Reoxidation Al 2 O 3
11 Case 1: Uncovering reaction mechanism by operando spectroscopy 1Sb 1 V/Al 8.8 ACN/V sec +48% 4.8 ACN/V sec 2Sb 5 V/Al Bañares et al., J.Mater.Chem.(2002) Surface vanadia on SbVO 4 species trigger conversion/selectivity specific rate
12 Málaga, March 243th, 2010 Case 1: Uncovering reaction mechanism by operando spectroscopy Propane activation 5+ Sb 2 O 4 VSbO 4 phases 5+ O V / \ O O O Redox cycle between surface V 5+ and bulk V 3+ sites Al 2 O 3 Ammoxidation Reoxidation
13 Case 1: Sb-V-O catalytic materials for propane ammoxidation VSbO 4 active phase succesfully nanoscaled on the surface of alumina support. Identified active species during propane ammoxidation by Raman spectroscopy. Reaction Mechanism proposed.
14 Case 2: Mo-V-Te-Nb-O catalytic materials for propane oxidation Acrylic acid useful chemical intermediate (fibers, polymers, resins. and much more) PROPYLENE PROPANE ACROLEIN TWO ONE STEPS ACRYLIC ACID
15 Case 2: Mo-V-Te-Nb-O catalytic materials for propane oxidation Previous studies: bulk catalysts M1 and rutile: active phases Grasselli et al. Guliants et al. Ueda et al. López Nieto et al.
16 Case 2: Synthesis of nanostructured catalysts 4MoVNbTe/Al 2 O 3 12MoVNbTe/Al 2 O 3 Bulk MoVNbTeO
17 Case 2: XRD patterns of Mo-V-Te-Nb catalysts MoO2 Rutile Mo-V-Nb M1 Al2O3 High coverage Low coverage Q
18 Case 2: Characterization of Mo-V-Te-Nb catalysts HRTEM confirms the presence of M1 phase
19 Conversion (%) or Selectivity (%) Nanospain Conference M. Olga Guerrero Pérez Case 2: Mo-V-Te-Nb-O catalytic materials for propane oxidation Supported catalysts performs better! % propane conversion % acrylic acid % acrolein % propylene % COx MoVNbTe rutile 4Mo5V4Nb0.5Te0.5 12Mo5V4Nb0.5Te0.5 Bulk Low coverage High coverage
20 Case 2: Mo-V-Te-Nb-O catalytic materials for propane oxidation Nanoscaled Rutile and M1 active phases have been succesfully supported on the surface of alumina. It is possible to obtain active and selective nanoscaled catalysts, that performs, even better, that the corresponding bulk catalysts.
21 Mo-V-Nb-Te-O for propane oxidation Sb-V-O for propane ammoxidation Rutile and M1 active phases It have been possible to obtain active and selective nanoscaled catalysts. Identification of active phase under reaction conditions.
22 Catalytic Spectroscopy Laboratory Instituto de Catálisis y Petroleoquímica, CSIC Ricardo López-Medina Miguel A. Bañares
23 Acknowledgements Spanish Ministry of Education and Science (CTQ /PPQ) MAEC-AECID Predoctoral fellowship (RLM) ESF (COST Action D )
24 Thank you very much for your attention!!!
25 Case 2: Raman spectra of Mo-V-Te-Nb catalysts VOx MoOx dispersed on alumina rutile M1 Mo-V-O High coverage MoO2 visible at low coverages Low coverage
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