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Preparation of titanocene and zirconocene dichlorides bearing bulky 1,4-dimethyl-2,3-diphenylcyclopentadienyl ligand and their behavior in polymerization of ethylene |
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| Authors: | Michal Horá ?ek,Jan Merna,Philippe Meunier |
| Affiliation: | a J. Heyrovský Institute of Physical Chemistry of ASCR, v.v.i., Dolejškova 2155/3, 182 23 Prague 8, Czech Republic b Institute of Chemical Technology, Prague, Department of Polymers, Technická 5, 166 28 Prague 6, Czech Republic c Charles University, Department of Inorganic Chemistry, Hlavova 2030, 128 40 Prague 2, Czech Republic d Institut de Chimie Moléculaire de l’Université de Bourgogne (ICMUB, UMR CNRS 5260), Université de Bourgogne, 9, Avenue Alain Savary, 21078 Dijon, France |
| Abstract: | New metallocene dichlorides [η5-(1,4-Me2-2,3-Ph2-C5H)2TiCl2] (2), [η5-(1,4-Me2-2,3-Ph2-C5H)2ZrCl2] (3) and [η5-(1,4-Me2-2,3-Ph2-C5H)η5-(C5H5)ZrCl2] (4) were prepared from lithium salt of 1,4-dimethyl-2,3-diphenylcyclopentadiene (1) and [TiCl3(THF)3], [ZrCl4] and [η5-(C5H5)ZrCl3(DME)], respectively. Compounds 2-4 were characterized by NMR spectroscopy, EI-MS and IR spectroscopy, and the solid state structure of 3 was determined by single crystal X-ray crystallography. The catalytic systems 3/MAO and 4/MAO were almost inactive in polymerization of ethylene at 30-50 °C, however, they exhibited high activity at temperature 80 °C. The catalyst formed from 2 and excess of MAO was practically inactive at all temperatures. |
| Keywords: | Substituted cyclopentadienes Titanocene Zirconocene Ethylene polymerization Crystal structure |
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