In Situ IR and X-ray High Spatial-Resolution Microspectroscopy Measurements of Multistep Organic Transformation in Flow Microreactor Catalyzed by Au Nanoclusters.

Analysis of catalytic organic transformations in flow reactors and detection of short-lived intermediates are essential for optimization of these complex reactions. In this study, spectral mapping of a multistep catalytic reaction in a flow microreactor was performed with a spatial resolution of 15...

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Publicado en:Journal of the American Chemical Society Vol. 136; no. 9; pp. 3624 - 3630
Autores principales: Gross, Elad, Xing-Zhong Shu, Alayoglu, Selim, Bechtel, Hans A., Martin, Michael C., Toste, F. Dean, Somorjai, Gabor A.
Formato: Artículo
Publicado: American Chemical Society 3/5/2014
Materias:
Acceso en línea:Ver este registro en EBSCOhost
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      dt: 3/5/2014
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      pub: American Chemical Society
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        95084500
        10.1021/ja412740p
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        atl: In Situ IR and X-ray High Spatial-Resolution Microspectroscopy Measurements of Multistep Organic Transformation in Flow Microreactor Catalyzed by Au Nanoclusters.
      aug:
        au:
          Gross, Elad
          Xing-Zhong Shu
          Alayoglu, Selim
          Bechtel, Hans A.
          Martin, Michael C.
          Toste, F. Dean
          Somorjai, Gabor A.
        affil:
          Department of Chemistry, University of California, Berkeley, California 94720, United States, and Chemical Sciences Division, Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, California 94720, United States
          Advanced Light Source, Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, California 94720, United States
      su:
        Gold nanoparticles
        Gold clusters
        Microreactors
        Synchrotrons
        Silica
        Mesoporous materials
        Pyran
        Biochemical substrates
      sug:
        subj:
          Gold nanoparticles
          Gold clusters
          Microreactors
          Synchrotrons
          Silica
          Mesoporous materials
          Pyran
          Biochemical substrates
      ab: Analysis of catalytic organic transformations in flow reactors and detection of short-lived intermediates are essential for optimization of these complex reactions. In this study, spectral mapping of a multistep catalytic reaction in a flow microreactor was performed with a spatial resolution of 15 μm, employing micrometer-sized synchrotron-based IR and X-ray beams. Two nanometer sized Au nanoclusters were supported on mesoporous SiO, packed in a flow microreactor, and activated toward the cascade reaction of pyran formation. High catalytic conversion and tunable products selectivity were achieved under continuous flow conditions. In situ synchrotron-sourced IR microspectroscopy detected the evolution of the reactant, vinyl ether, into the primary product, allenic aldehyde, which then catalytically transformed into acetal, the secondary product. By tuning the residence time of the reactants in a flow microreactor a detailed analysis of the reaction kinetics was performed. An in situ micrometer X-ray absorption spectroscopy scan along the flow reactor correlated locally enhanced catalytic conversion, as detected by IR microspectroscopy, to areas with high concentration of Au(III), the catalytically active species. These results demonstrate the fundamental understanding of the mechanism of catalytic reactions which can be achieved by the detailed mapping of organic transformations in flow reactors.
      pubtype: Academic Journal
      doctype: Article
      src: R
    language: English
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          year: 2014
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