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Solid state 13C NMR characterisation study on fourth generation Ziegler-Natta catalysts.

Harri Heikkinen¹, Tiina Liitiä, Ville Virkkunen

¹VTT Technical Research Centre of Finland, Biologinkuja 7, Espoo, PO Box 1000 02044 VTT, Finland. harri.heikkinen@vtt.fi

Solid State Nuclear Magnetic Resonance

|March 20, 2012

Summary

Solid-state carbon-13 NMR spectroscopy identified metal-ester coordination in Ziegler-Natta catalysts. This research provides molecular insights into how internal donors interact with active species in these phthalate-based systems.

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Area of Science:

Catalysis
Polymer Chemistry
Spectroscopy

Background:

Ziegler-Natta catalysts are crucial for olefin polymerization.
Internal donors influence the active species in Ziegler-Natta catalysts.
Limited molecular-level data exists on donor-active species interactions.

Purpose of the Study:

To characterize metal-ester coordination in fourth-generation Ziegler-Natta catalysts.
To elucidate the interplay between internal donors and active species.
To gain detailed molecular insights into catalyst active sites.

Main Methods:

Solid-state carbon-13 Nuclear Magnetic Resonance (NMR) spectroscopy.
Low magic-angle spinning (MAS) NMR for anisotropy tensor values (δ(11), δ(22), δ(33)).
Chemical shift anisotropy (CSA) calculations (δ(aniso) and η) for symmetry analysis.

Main Results:

Successfully identified metal-ester coordination in phthalate-based Ziegler-Natta catalysts.
Determined the coordinative metal species (Mg/Ti) involved in the active sites.
Characterized the symmetry of metal-donor interactions within the catalyst system.

Conclusions:

Solid-state (13)C NMR spectroscopy is effective for characterizing Ziegler-Natta catalysts.
Detailed molecular information on donor-active species interactions was obtained.
The study enhances understanding of catalyst structure-activity relationships.