Understanding the leaching properties of heterogenized catalysts: A combined solid-state and PHIP NMR study

作者:Gutmann Torsten; Ratajczyk Tomasz; Xu Yeping; Breitzke Hergen; Gruenberg Anna; Dillenberger Sonja; Bommerich Ute; Trantzschel Thomas; Bernarding Johannes; Buntkowsky Gerd*
来源:Solid State Nuclear Magnetic Resonance, 2010, 38(4): 90-96.
DOI:10.1016/j.ssnmr.2011.03.001

摘要

Para-hydrogen induced polarization (PHIP) NMR in solution, combined with solid-state NMR, can be efficiently employed for the highly sensitive in-situ detection of the leaching properties of immobilized catalysts. The knowledge of this property is important for possible applications of PHIP experiments in medicine, biology or industry, where leached catalysts poison the solution of hyperpolarized products. As experimental example Wilkinson's catalyst RhCl(PPh3)(3) (1) immobilized on mesoporous silica is chosen. As model reaction the hydrogenation of styrene in solvents with different polarities (methanol-d(4), acetone-d(6) and benzene-d(6)) is used. A P-31 solid-state MAS-NMR study reveals that there are two different species of catalysts on the silica, namely coordinatively bound catalysts and physisorbed catalyst. Only the second species exhibits substantial leaching, which is visible in a strong PHIP enhancement of the reaction product.

  • 出版日期2010-11