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Immobilization of η-cyclopentadienyltris(dimethylamido)zirconium polymerization catalysts on a chlorosilane- and HMDS-modified mesoporous silica surface: a new concept for supporting metallocene amides towards heterogeneous single-site-catalysts |
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| Authors: | Horst Schneider Gerd T Puchta Franz A R Kaul Gabriele Raudaschl-Sieber Frdric Lefebvre Guillaume Saggio Dimitrios Mihalios Wolfgang A Herrmann Jean Marie Basset |
| Institution: | a Lehrstuhl für Anorganische Chemie, Anorganisch-Chemisches Institut, Technische Universität München, Lichtenbergstr. 4, 85747 Garching, Germany b Laboratoire de Chimie Organométallique de surface UMR CNRS-CPE 9986, 43 Bd du 11 novembre 1918, 691616 Villeurbanne Cedex, France |
| Abstract: | The modification of a mesoporous silica surface with Si(Ind)(CH3)2Cl and the immobilization of CpZr(NMe2)3 on this surface was studied via IR-spectroscopy. To reduce side reactions, the indenyl-modified silica was reacted with hexamethyldisilazane (HMDS) under IR-control before the CpZr(NMe2)3-immobilization. The role of the hydroxyl group protection with HMDS is discussed. The surface modifications have been repeated via Schlenk technique at the same conditions and the surface modifications were studied with 13C CP MAS–NMR, 1H MAS–NMR, elemental-, SEM- and BET-analysis. The surface species of the resulting catalysts are discussed. The precatalysts have been treated with methylaluminoxane (MAO) (Al:Zr (mol:mol)=500:1) and the resulting Zr contents (leaching-effect) are discussed. All catalysts have been tested in ethylene and propylene polymerization. |
| Keywords: | Heterogeneous catalysts Metallocene Polymerization Surface chemistry Leaching |
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