Gutmann, T. and Ratajczyk, T. and Xu, Y. P. and Breitzke, H. and Grünberg, A. and Dillenberger, S. and Bommerich, U. and Trantzschel, T. and Bernarding, J. and Buntkowsky, G. (2010):
Understanding the leaching properties of heterogenized catalysts: A combined solid-state and PHIP NMR study.
38, In: Solid State Nuclear Magnetic Resonance, (4), pp. 90-96. [Article]
Abstract
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. (C) 2011 Elsevier Inc. All rights reserved.
| Item Type: | Article |
|---|---|
| Erschienen: | 2010 |
| Creators: | Gutmann, T. and Ratajczyk, T. and Xu, Y. P. and Breitzke, H. and Grünberg, A. and Dillenberger, S. and Bommerich, U. and Trantzschel, T. and Bernarding, J. and Buntkowsky, G. |
| Title: | Understanding the leaching properties of heterogenized catalysts: A combined solid-state and PHIP NMR study |
| Language: | English |
| Abstract: | 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. (C) 2011 Elsevier Inc. All rights reserved. |
| Journal or Publication Title: | Solid State Nuclear Magnetic Resonance |
| Volume: | 38 |
| Number: | 4 |
| Uncontrolled Keywords: | phip solid-state nmr mas wilkinson's catalyst immobilization parahydrogen-induced polarization hydrogen-induced polarization in-situ homogeneous hydrogenation wilkinsons catalyst stereoselective hydrogenation cyclohexene hydroformylation metal-complexes silica olefins |
| Divisions: | 07 Department of Chemistry 07 Department of Chemistry > Physical Chemistry |
| Date Deposited: | 27 Oct 2014 20:41 |
| Official URL: | http://apps.webofknowledge.com/full_record.do?product=WOS&se... |
| Additional Information: | 755VB Times Cited:9 Cited References Count:62 |
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