Double-Chamber Flow Cell for in Situ Infrared Spectroscopy Studies of Chemical Reactions in Ziegler-Natta Catalyst Systems

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A complete experimental setup for in situ infrared transmission spectroscopy studies of solid/liquid reactions in Ziegler-Natta catalysts has been developed. The main part of the apparatus, the flow cell, facilitates separate recording of the liquid-phase spectrum and the superimposed solid/liquid spectrum, and thus allows solid and dissolved species during reactions to be distinguished. Addition of solutes and exchange of solution during the experiments are made possible, thus allowing subsequent reactions to be studied. The setup is suited also for liquid reactions, and, in principle, for other chemical systems as well. The construction of the flow cell and the operation conditions are based on pressure-drop calculations of the flow in the apparatus. Two experimental studies are included to demonstrate the use and to document the performance of the setup: (1) the reaction of MgCl2 with dissolved ethyl benzoate and AlEt3 in succession, and (2) the interaction of a MgCl2/ethyl benzoate support during TiCl4 treatment. In the latter, a hitherto unknown TiCl4/EB complex is discovered in the TiCl4 solution.

Keywords: In situ infrared spectroscopy; Reaction flow cell; Ziegler-Natta catalysis

Document Type: Research Article


Affiliations: Department of Inorganic Chemistry, Norwegian Institute of Technology, NTH, N-7034 Trondheim, Norway

Publication date: August 1, 1994

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