Integration of reaction and separation in a micro-capillary column reactor

• Verfasst von: Weber, Sven K. [VerfasserIn]
• Verfasst von: Bremer, Sabrina [VerfasserIn]
• Verfasst von: Trapp, Oliver [VerfasserIn]
• Titel: Integration of reaction and separation in a micro-capillary column reactor
• Titelzusatz: palladium nanoparticle catalyzed C-C bond forming reactions
• Verf.angabe: Sven K. Weber, Sabrina Bremer, Oliver Trapp
• Jahr: 2010
• Umfang: 7 S.
• Illustrationen: Illustrationen
• Fussnoten: Online veröffentlicht am 8. September 2009 ; Gesehen am 17.10.2023
• Titel Quelle: Enthalten in: Chemical engineering science
• Ort Quelle: Amsterdam [u.a.] : Elsevier Science, 1951
• Jahr Quelle: 2010
• Band/Heft Quelle: 65(2010), 7, Seite 2410-2416
• DOI: doi:10.1016/j.ces.2009.09.006
• Datenträger: Online-Ressource
• Sprache: eng
• Sach-SW: C-C cross-coupling
• Sach-SW: Catalysis
• Sach-SW: Chemical analysis
• Sach-SW: Chemical reactors
• Sach-SW: Chromatography
• Sach-SW: Multiphase reactions
• Sach-SW: On-column reaction chromatography
• Sach-SW: Palladium nanoparticles
• K10plus-PPN: 1865943487

Abstract

The Ullmann-type coupling C-C cross-coupling reactions of different aromatic halides over highly active Pd nanoparticles embedded in a polycyanoethylphenyl methylsiloxane was studied by on-column reaction gas chromatography. In these experiments, catalysis and separation of educts and products are integrated by the use of a catalytically active gas chromatographic stationary phase, which allows very efficiently the measurement of reaction rate measurements by employing reactant libraries. Here the polysiloxane, used as stationary phase, was modified with catalytically highly active Pd nanoparticles and coated as a thin film of 500nm onto the inner surface of the micro-capillary with an inner diameter of 250μm and serves both as solvent and selective stationary phase to allow the synchronous combination of catalysis and separation in a gas chromatographic reactor. Besides the biarylation reaction of aryl halides we observed the cyanation by transfer of nitrile-groups from the polysiloxane matrix in the presence of the Pd nanoparticles. Herein, we demonstrate by systematic on-column reaction chromatographic measurements and TEM investigations the synthetic applicability of multiphase (gas-liquid-solid) C-C cross-coupling as well as cyanation reactions in micro-capillary reactors.