Supported high activity polyolefin catalyst component with regular distribution of magnesium values provided utilizing a controlled drying protocol

• US 5,275,991 A
• Filed: 11/30/1992
• Issued: 01/04/1994
• Est. Priority Date: 09/21/1987
• Status: Expired due to Fees

• Current Assignee: Equistar Chemicals LP (Lyondellbasell Industries NV)
• Original Assignee: Quantum Chemical Corporation (Heidelberg Materials AG)
• Inventors: Masino, Albert P., Buehler, Charles K., Menon, Raghu
• Primary Examiner(s): GARVIN, PATRICK
• Application Number:
  US07/984,052
• Time in Patent Office: 400 Days
• Field of Search: 502/104, 502/107, 502/111, 502/112, 502/103, 502/120, 502/125
• US Class Current: 502/107
• CPC Class Codes: C08F 10/00 Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
• CPC Class Codes: C08F 4/6545 and metals of C08F4/64 or compounds thereof
• CPC Class Codes: C08F 4/6555 and magnesium or compounds thereof
• CPC Class Codes: C08F 4/6565 and magnesium or compounds thereof
• CPC Class Codes: C08F 4/6567 and aluminium or compounds thereof
• CPC Class Codes: C08F 4/6574 and magnesium or compounds thereof
• CPC Class Codes: C08F 4/6578 and silicon or compounds thereof

Abstract

A novel catalyst support and a method for preparation thereof, characterized by the presence of selected amounts of a hydrocarbon soluble magnesium-containing compound applied to the support relative to solvent, wherein a surface uniformly and essentially continuously moistened with the solvated magnesium compound in a condition of incipient precipitation to permit the formation of a regular essentially continuous distribution of the magnesium compound onto and conforming to the support material. The drying process under these conditions is effective in maintaining to a high degree the effective surface area and pore volume of the material. The support containing the adsorbed magnesium is then dried in a controlled manner to essential incipient wetness conditions providing a regular spatial distribution of stacked reticular magnesium values at a level of one to five molecular monolayers on the support.

A representative process for polymerizing or copolymerizing olefins providing stereospecific polymers such as propylene is disclosed.

Claims

1. In a method of preparing a supported catalyst component for the polymerization of at least one alpha olefin, including the steps of effecting interaction between a hydrocarbon soluble magnesium compound solubilized in a hydrocarbon solvent with an inorganic catalyst support including applying said magnesium compound in said solvent to said support, and drying the so-treated support to concentrate the solution, the improvement which comprises effecting such drying so to remove a selected proportion of said solvent and effect the formation of a regular spatial distribution of magnesium values in and upon the effective surface area of said inorganic support, wherein the magnesium value upon the completion of the drying step is from about 0.1 to about 12 weight percent of magnesium to inorganic support.

2. The method of claim 1 wherein the solvent is removed at a rate of about 0.05 to about 5.0 g solvent/g support/hr.

3. The method of claim 2 wherein the solvent is removed at a rate of about 0.1 to about 2.0 g of solvent/g support/hr.

4. The method of claim 1 wherein n said drying step removes from about 20 to about 80 wt % of the initial quantity of solvent.

5. The method of claim 4 wherein said drying step removes about 30 to about 70 wt % of the initial quantity of solvent.

6. The method of claim 1 wherein the inorganic support is silica.

7. The method of claim 1 wherein the hydrocarbon soluble magnesium compound is an alkoxymagnesium halide.

8. The method of claim 7 wherein the solution of alkoxymagnesium halide in said hydrocarbon solvent is near or at saturation.

9. The method of claim 1 wherein said solvent is heptane.

10. The method of claim 9 wherein said alkoxymagnesium halide is an alkoxymagnesium chloride.

11. The method of claim 9 wherein said alkoxymagnesium halide is 2-methyl 1-pentyloxy magnesium chloride.

12. The method of claim 9 wherein said alkoxymagnesium halide is associated with 0.5 to 1.5 moles/mole of an alcohol corresponding to the alkyl moiety of the alkoxy group.

13. The method of claim 12 wherein the drying process is effective in removing from about 0.1 to about 2% of the associated alcohol.

14. The method of claim 13 wherein the drying process effective in removing about 0.5% of the associated alcohol.

15. A particulate, granular catalyst component useful for preparing a catalyst for the polymerization of alpha olefins to stereospecific polymers of high bulk density and high heptane insolubles with high yield and activity comprising a high surface area/high pore volume silica support impregnated with an alkoxymagnesium halide regularly microdistributed thereon in an amount sufficient to provide 0.1 to 10 weight percent of magnesium in and upon said support, and the treated surface of the support being essentially uniformly wetted with solvent after removal of a portion of said solvent

16. The catalyst component of claim 15 wherein the support contains up to 80% solvent.

17. The catalyst component of claim 16 wherein the support from 30 to 70% solvent.

18. The catalyst component of claim 17 wherein from 98 to 100% of the alcohol content associated with the alkoxymagnesium halide compound is present on the support.

19. The catalyst component of claim 15 wherein the dried silica has a surface area of about 80 to 400 m² /g, more preferably 100 to 350 and a pore volume of about 0.3 to 1.5, more preferably 0.6 to 1.0 ml/g.

20. The catalyst component of claim 15 further reacted with at least one or more titanium compound having the structural formula TiX_n Y_4-n where X is Cl, Br, I;

Y=F, R, OR or NR₂ wherein R=C₁ to C₁₂ hydrocarbyl;

n is 0 or an integer from 1 to 4.

21. The catalyst component of claim 20 wherein said titanium compound is a titanium tetraalkoxide.

22. The catalyst component of claim 20 wherein said titanium compound is a titanium tetraalkoxide.

24. The catalyst component of claim 15 wherein said alkoxymagnesium halide is associated with 0.5 to 1.5 moles/mole of an alcohol corresponding to the alkyl moiety of the alkoxy group.

23. A catalyst component for the polymerization of propylene and alpha olefin monomers copolymerizable therewith comprising an inorganic support of high surface area and pore volume treated with an alkoxy magnesium halide compound and a titanium halide, wherein the alkoxymagnesium halide values are distributed in and upon the surface of said inorganic support responsive to the controlled removal of solvent for said magnesium compound to provide a residual regularly distributed population of magnesium values of from about 0.05 to about 12 weight percent of magnesium to silica.