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High-throughput kinetic study of hydrogenation over palladium nanoparticles: combination of reaction and analysis : Eine Kombination aus Reaktion und Analyse bei der kinetischen Untersuchung der Hydrierung auf feinteiligen Palladium-Partikeln

For the directed design of catalysts, comprehensive kinetic and thermodynamic data of existing catalytic systems are necessary to understand how the catalytic mechanism might be controlled by structural parameters. A major drawback of commonly used batch reactors is the limitation of studying only o... Full description

Contained in: Chemistry - A European Journal Vol. 14, No. 15 (2008), p. 4657-4666
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Links: Additional Link (dx.doi.org)
ISSN: 1521-3765
Additional Keywords: GASCHROMATOGRAPHIE
HYDRIEREN
MORPHOLOGIE
NANOPARTIKEL
PALLADIUM
REAKTIONSKINETIK
SILICON:POLYMER
TRANSMISSIONSELEKTRONENMIKROSKOPIE
DOI: 10.1002/chem.200701780
Notes: Copyright: Metadaten: TEMA, Copyright WTI-Frankfurt eG
Copyright: (C) Alle Rechte beim Herausgeber
Physical Description: 10 Seiten, 17 Bilder, 4 Tabellen, 84 Quellen
ID (e.g. DOI, URN): 10.1002/chem.200701780
PPN (Catalogue-ID): WTI045710058
Note: WTI TEMA DB
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520 |a For the directed design of catalysts, comprehensive kinetic and thermodynamic data of existing catalytic systems are necessary to understand how the catalytic mechanism might be controlled by structural parameters. A major drawback of commonly used batch reactors is the limitation of studying only one reaction per run. Recently, the authors of this contribution reported a strategy that allows the synchronous combination of catalysis and separation in capillaries to perform high-throughput reaction rae measurements of reactant libraries for hydrogenation over highly active palladium nanoparticles. The hydrogenation of 1-acetylcyclohexene, cyclohex-2-enone, nitrobenzene, and trans-methylpent-3-enoate catalyzed by highly active palladium nanoparticles was studied by high-throughput on-column reaction gas chromatography. In these experiments, catalysis and separation of educts and products is integrated by the use of a catalytically active gas chromatographic stationary phase, which allows reaction rate measurements to be efficiently performed by employing reactant libraries. Palladium nanoparticles embedded in a stabilizing polysiloxane matrix serve as catalyst and selective chromatographic stationary phase for these multiphase reactions (gas-liquid-solid) and are coated in fused-silica capillaries (inner diameter 250 mu m) as a thin film of thickness 250 nm. The palladium nanoparticles were prepared by reduction of palladium acetate with hydridomethylsiloxane-dimethylsiloxane copolymer and self-catalyzed hydrosilylation with methylvinylsiloxane-dimethylsiloxane copolymer to obtain a stabilizing matrix. Diphenylsiloxane-dimethylsiloxane copolymer (GE SE 52) was added to improve film stability over a wide range of compositions. Herein, we show by systematic TEM investigations that the size and morphology (crystalline or amorphous) of the nanoparticles strongly depends on the ratio of the stabilizing polysiloxanes, the conditions to immobilize the stationary phase on the surface of the fused-silica capillary, and the loading of the palladium precursor. Furthermore, hydrogenations were performed with these catalytically active stationary phases between 60 and 100 C at various contact times to determine the temperature-dependent reaction rate constants and to obtain activation parameters and diffusion coefficients. [Copyright Wiley-VCH Verlag GmbH & Co. KGaA. Reproduced with permission.] 
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653 4 |a SILICON:POLYMER 
653 4 |a TRANSMISSIONSELEKTRONENMIKROSKOPIE 
653 4 |a MORPHOLOGIE 
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