Palladium(0) Nanoparticles on Glass‐Polymer Composite Materials as Recyclable Catalysts: A Comparison Study on their Use in Batch and Continuous Flow Processes

Advanced Synthesis and Catalysis - Tập 350 Số 5 - Trang 717-730 - 2008
Klaas Mennecke1, R. Cecilia2, Toma N. Glasnov3, S. Gruhl4, Carla Vogt4, Armin Feldhoff5, M.Á. Larrubia6, C. Oliver Kappe3, Ulrich Kunz2, Andreas Kirschning1
1Center of Biomolecular Drug Research (BMWZ) and Institute of Organic Chemistry, Leibniz Universität Hannover, Schneiderberg 1B, 30167 Hannover, Germany, Fax: (+49)‐511‐762‐3011
2Institute of Chemical Process Engineering (ICVT), Clausthal University of Technology, Leibnizstr. 17, 38678 Clausthal‐Zellerfeld, Germany
3Christian Doppler Laboratory for Microwave Chemistry and Institute of Chemistry, Karl Franzens University, Heinrichstraβe 28, 8010 Graz, Austria
4Institute of Inorganic Chemistry, Leibniz Universität Hannover, Callinstraße 9, 30167 Hannover, Germany
5Institute of Physical Chemistry and Electrochemistry Leibniz Universität Hannover Callinstraße 3–3a 30167 Hannover Germany
6Chemical Engineering Department, University of Malaga, Campus de Teatinos, 29071 Malaga, Spain

Tóm tắt

AbstractPalladium particles were generated by reduction of palladate anions bound to an ion exchange resin inside microreactors. The size and distribution of the palladium particles differed substantially depending on the degree of cross‐linking and the density of ion exchange sites on the polymer/glass composites, the latter parameter having a larger influence than the former. The polymer phase of the composite materials was used for the loading with clusters composed of palladium particles which are 1 to 10 nm in diameter. The reactivity and stability of six different palladium‐doped polymer/glass composite samples for transfer hydrogenations was investigated both under conventional and microwave heating in the batch mode as well as under continuous flow conditions using the cyclohexene‐promoted transfer hydrogenation of ethyl cinnamate as a model reaction. Regarding the heating method it was found that catalysts that are composed of larger metal particles perform better under microwave irradiating conditions whereas samples with smaller particle sizes perform better under conventional heating. Comparing batch experiments with flow‐through experiments the latter technique gives better conversion. Reusability was better in microwave heated experiments than in traditional heating.

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