WO2002079209A1 - Titanocene synthesis - Google Patents
Titanocene synthesis Download PDFInfo
- Publication number
- WO2002079209A1 WO2002079209A1 PCT/US2002/004164 US0204164W WO02079209A1 WO 2002079209 A1 WO2002079209 A1 WO 2002079209A1 US 0204164 W US0204164 W US 0204164W WO 02079209 A1 WO02079209 A1 WO 02079209A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- titanium
- complex
- titanocene
- titanium trichloride
- reagent
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F17/00—Metallocenes
Definitions
- This invention relates to titanium-trihalide complexes free from contamination with salts of metals other than titanium. More particularly, the invention relates to the synthesis of such adducts and to the conversion thereof to titanocenes.
- BACKGROUND OF THE INVENTION Application Serial No. 09/784,736 describes a method for converting a Ti(IV) compound to a complex of a Ti(III) compound free of foreign metal contaminations .
- a preferred embodiment of the invention entails the reduction of TiCl 4 with particulate titanium in the presence of a reagent which forms a titanium trichloride complex insoluble in the reduction reaction mixture. According to that application, the consequent titanium trichloride complex may be converted to a titanocene in known manner. See, e.g., United States patent 6,218,557. SUMMARY OF THE INVENTION
- This invention provides methods for the conversion to titanocenes of the titanium trichloride complex as described in application Serial No. 09/784,736. DETAILED DESCRIPTION OF THE INVENTION
- the invention may comprise a first step in which a titanium trichloride complex free of contamination with salts of other metals is produced.
- a second step of this invention may comprise treatment of a ligand with the titanium trichloride complex product of the first step to produce a titanocene.
- One example illustrative of the first step is to charge a flask with particulate titanium ( ⁇ 100 mesh, 0.25 mole, 11.9 g) and dimethoxyethane (DME) (2 kg).
- Product is aluminum and magnesium free.
- the reduction reaction may optionally be conducted in a medium comprising the complex-forming reagent per se or in such combination with any non- interfering medium.
- Suitable media include aliphatic and aromatic hydrocarbons; aromatic hydrocarbons are preferred.
- Another aspect of the invention may include conversion of the Ti(III) complexes to metallocenes, which are also free of contamination with the salts of metals other than titanium, useful as olefin polymerization catalyst ligands, as olefin polymerization catalysts per se, or as components of olefin polymerization catalyst systems .
- EXAMPLE 2 This example is a general illustration of the second step of the invention. The TiCl 3 *DME complex as produced in Example 1 is used instead of the TiCl 3 per se in each or any of the relevant examples of United States patent 6,218,557 to produce a titanocene.
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA002405989A CA2405989A1 (en) | 2001-02-15 | 2002-02-13 | Titanocene synthesis |
JP2002577833A JP2004519517A (en) | 2001-02-15 | 2002-02-13 | Titanocene synthesis |
EP02724934A EP1360188A4 (en) | 2001-02-15 | 2002-02-13 | Titanocene synthesis |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US09/784,736 | 2001-02-15 | ||
US09/784,736 US6307063B1 (en) | 2001-02-15 | 2001-02-15 | Conversion of compounds of titanium in a plus 4 oxidation state to titanium compounds in a plus 3 oxidation state |
US09/880,289 US6444835B1 (en) | 2001-02-15 | 2001-06-13 | Titanocene synthesis |
US09/880,289 | 2001-06-13 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2002079209A1 true WO2002079209A1 (en) | 2002-10-10 |
Family
ID=27120329
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2002/004164 WO2002079209A1 (en) | 2001-02-15 | 2002-02-13 | Titanocene synthesis |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP1360188A4 (en) |
JP (1) | JP2004519517A (en) |
CA (1) | CA2405989A1 (en) |
WO (1) | WO2002079209A1 (en) |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5264950A (en) * | 1992-01-06 | 1993-11-23 | Kent State University | Light modulating device with polarizer and liquid crystal interspersed as spherical or randomly distorted droplets in isotropic polymer |
US5367085A (en) * | 1993-09-20 | 1994-11-22 | Albemarle Corporation | Preparation of TiCl3 coordination complexes |
DE19739946A1 (en) * | 1997-09-11 | 1999-03-18 | Targor Gmbh | Process for the production of metallocenes |
US6093833A (en) * | 1999-01-14 | 2000-07-25 | Akzo Nobel N.V. | Process for producing trivalent titanium coordination complex |
US6218557B1 (en) * | 1996-11-22 | 2001-04-17 | Boulder Scientific Company | Synthesis of titanocenes |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SU941294A1 (en) * | 1980-04-18 | 1982-07-07 | Донецкий Ордена Трудового Красного Знамени Политехнический Институт | Process for producing titanium trichloride |
-
2002
- 2002-02-13 WO PCT/US2002/004164 patent/WO2002079209A1/en active Application Filing
- 2002-02-13 CA CA002405989A patent/CA2405989A1/en not_active Abandoned
- 2002-02-13 JP JP2002577833A patent/JP2004519517A/en active Pending
- 2002-02-13 EP EP02724934A patent/EP1360188A4/en not_active Withdrawn
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5264950A (en) * | 1992-01-06 | 1993-11-23 | Kent State University | Light modulating device with polarizer and liquid crystal interspersed as spherical or randomly distorted droplets in isotropic polymer |
US5367085A (en) * | 1993-09-20 | 1994-11-22 | Albemarle Corporation | Preparation of TiCl3 coordination complexes |
US5367085B1 (en) * | 1993-09-20 | 1997-02-25 | Albermarle Corp | Preparation of TiCl3 coordination complexes |
US6218557B1 (en) * | 1996-11-22 | 2001-04-17 | Boulder Scientific Company | Synthesis of titanocenes |
DE19739946A1 (en) * | 1997-09-11 | 1999-03-18 | Targor Gmbh | Process for the production of metallocenes |
US6093833A (en) * | 1999-01-14 | 2000-07-25 | Akzo Nobel N.V. | Process for producing trivalent titanium coordination complex |
Non-Patent Citations (1)
Title |
---|
See also references of EP1360188A4 * |
Also Published As
Publication number | Publication date |
---|---|
EP1360188A4 (en) | 2007-03-07 |
CA2405989A1 (en) | 2002-10-10 |
EP1360188A1 (en) | 2003-11-12 |
JP2004519517A (en) | 2004-07-02 |
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