Preparation of titanium (II) or zirconium (II) complexes
AssigneeThe Dow Chemical Company
InventorsRobert K. Rosen, Brian W. S. Kolthammer
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Abstract
Titanium and zirconium complexes comprising a single, cyclic, delocalized n-bonded ligand group wherein the metal of said complexes is in the +2 formal oxidation state are prepared in high yield and purity by reaction of titanium and zirconium halides in the +3 or +4 oxidation state with an n-alkyl Grignard reagent. The complexes are used as catalyst components for .alpha.-olefin polymerization catalysts.
Claims13
A process for preparing a metal complex containing one and only one cyclic, delocalized n-bonded group, said complex corresponding to the formula:
- ##STR10## wherein, M is titanium or zirconium in the +2 formal oxidation state;
- L is a group containing a cyclic, delocalized, anionic, n-system through which the group is bound to M, and which group is also bound to Z;
- Z is a moiety bound to M via a .sigma.-bond, comprising boron, or a member of Group 14 of the Periodic Table of the Elements, and also comprising nitrogen, phosphorus, sulfur or oxygen, said moiety having up to 60 non-hydrogen atoms;
- X is a neutral, conjugated diene, optionally substituted with one or more hydrocarbyl groups, said X having up to 40 carbon atoms and forming a n-complex with M;
- X' is a neutral Lewis base ligand selected from amines, phosphines and ethers said X' having from 3 to 20 non-hydrogen atoms;
- and
- n is a number from 0 to 3;
- said process comprising contacting a metal halide compound corresponding to the formula ##STR11## wherein, M* is titanium or zirconium in the +3 formal oxidation state;
- M** is titanium or zirconium in the +4 formal oxidation state;
- X* is halide;
- and
- L, Z, X' and n are as previously defined;
- with a free diene corresponding to X, and subsequently or simultaneously contacting the resulting reaction mixture with a Grignard derivative of a C.sub.1-20 n-alkane to form the desired metal complex.
A process for preparing a metal complex containing one and only one cyclic, delocalized n-bonded group, said complex corresponding to the formula:
- ##STR12## wherein, M is titanium or zirconium in the +2 formal oxidation state;
- L is a group containing a cyclic, delocalized, anionic, n-system through which the group is bound to M, and which group is also bound to Z;
- Z is a moiety bound to M via a .sigma.-bond, comprising boron, or a member of Group 14 of the Periodic Table of the Elements, and also comprising nitrogen, phosphorus, sulfur or oxygen, said moiety having up to 60 non-hydrogen atoms;
- X is a neutral, conjugated diene, optionally substituted with one or more hydrocarbyl groups, said X having up to 40 carbon atoms and forming a n-complex with M;
- X' is a neutral Lewis base ligand selected from amines, phosphines and ethers said X' having from 3 to 20 non-hydrogen atoms;
- and
- n is a number from 0 to 3;
- said process comprising:
- 1) contacting a metal halide compound according to the formula M*(X*).sub.3 X'.sub.n or M**(X*).sub.4 X'.sub.n, wherein;
- M* is titanium or zirconium in the +3 formal oxidation state;
- M** is titanium or zirconium in the +4 formal oxidation state;
- and
- X* is halide;
- with a dianionic salt corresponding to the formula:
- M'.sub.2 LZ, wherein;
- M' is a Group 1 metal, MgCl or MgBr or two M' groups together are a Group 2 metal;
- to form an intermediate metal complex according to the formula:
- ##STR13## wherein L, Z, M** , X*, X', M* and n are as previously defined;
- 2) when the metal in said intermediate metal complex is in the +3 formal oxidation state, optionally contacting said intermediate metal complex with an oxidant to form an intermediate metal complex according to the formula:
- ##STR14## wherein L, Z, M**, X*, X' and n are as previously defined;
- and 3) contacting the intermediate metal complex with a free diene corresponding to X, and subsequently or simultaneously contacting the resulting reaction mixture with a Grignard derivative of a C.sub.1-20 n-alkane to form the desired metal complex.
Dependencies are inferred from the claim text.