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Preparation of metallocene catalyst

A metallocene catalyst, metallocene technology, applied in metallocene, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of reducing polymer crystallinity, reducing syndiotacticity, etc. The effect of the dirt phenomenon

Inactive Publication Date: 2002-09-25
FINA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Likewise, any deviation or inversion within the chain structure reduces the syndiotacticity and thus the crystallinity of the polymer

Method used

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  • Preparation of metallocene catalyst
  • Preparation of metallocene catalyst
  • Preparation of metallocene catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] The preparation of embodiment 1 miPP catalyst

[0078] 5 g of MAO on P-10 silica was added to a 100 mL round bottom flask containing 30 mL of toluene and the flask was allowed to cool to 15°C. In a 20mL Wheaton bottle, the rac-Me 2 Si(2-Me-4-PhInd) 2 ZrCl 2 (65 mg) was slurried with 10 mL of toluene. This metallocene slurry was applied to a stirred dispersion of MAO on silica. The transfer of the metallocene was accomplished with a second 10 mL portion of toluene. The metallocene was reacted with MAO / silica at 15°C for 1 hour. After the solids had settled, the supernatant was removed with a cannula. Wash the loaded wet catalyst with 50 mL of toluene, let the solid settle, and take out the upper liquid with a cannula. Then, the supported wet catalyst was washed with 3 portions of 50 mL of hexane at 0° C. for 3 times. After the third hexane decantation, the wet catalyst slurry was diluted with 45 g of mineral oil. The miPP supported catalyst was obtained as a slu...

Embodiment 2

[0079] The preparation of embodiment 2 miPP catalyst

[0080] 4 g of MAO on P-10 silica was added to a 100 mL round bottom flask containing 30 mL of toluene and the flask was cooled to 0°C. In a 20mL Wheaton bottle, the rac-Me 2 Si(2-Me-4, 5-BzInd) 2 ZrCl 2 (60 mg) was slurried with 10 mL of toluene. This metallocene slurry was applied to a stirred dispersion of MAO on silica. The transfer of the metallocene was accomplished with a second 10 mL portion of toluene. The metallocene was reacted with MAO / silica at 0 °C for 1 hour. After the solids had settled, the supernatant was removed with a cannula. The supported wet catalyst was washed three times with 3 portions of 50 mL of hexane in sequence. After the third hexane decantation, the wet catalyst slurry was diluted with 45 g of mineral oil. A 7.0% solids slurry of the miPP supported catalyst was obtained.

Embodiment 3

[0081] The preparation of embodiment 3 miPP catalyst

[0082]4.8 g of MAO on P-10 silica was added to a 100 mL round bottom flask with 30 mL of toluene and the flask was cooled to 0°C. In a 20mL Wheaton bottle, the rac-Me 2 Si(2-MeInd) 2 ZrCl 2 (71 mg) was slurried with 10 mL of toluene. This metallocene slurry was applied to a stirred dispersion of MAO on silica. The transfer of the metallocene was accomplished with a second 10 mL portion of toluene. The metallocene was reacted with MAO / silica at 0 °C for 1 hour. After the solids had settled, the supernatant was removed with a cannula. The loaded wet catalyst was washed with 50 mL of hexane, and after the solid was allowed to settle, the upper liquid was taken out with a cannula. The supported wet catalyst was washed three times sequentially with 3 portions of 50 mL of hexane at 0°C. After the third hexane decantation, the wet catalyst slurry was diluted with 45 g of mineral oil. A 7.5% solids slurry of the miPP supp...

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Abstract

Process of preparing silica-supported catalysts. A support material comprising silica particles impregnated with an alumoxane co-catalyst with at least one-half of the co-catalyst disposed within the internal pore volume of the silica is contacted with a dispersion of a metallocene catalyst in an aromatic solvent. The dispersion and support are mixed at a temperature of about 10 DEG C or less to enable the metallocene to become reactively supported on and impregnated within the alumoxane-impregnated silica particles. The supported catalyst is recovered from the aromatic solvent and washed with an aromatic hydrocarbon and then a paraffinic hydrocarbon at a temperature of about 10 DEG C or less. The washed catalyst is dispersed in a viscous mineral oil.

Description

field of invention [0001] This invention relates to supported stereorigid metallocene catalyst systems for polymerizing ethylenically unsaturated compounds, and more particularly to a process for the preparation of supported metallocene catalysts using macroporous silica supports. background of the invention [0002] Many catalyst systems for polymerizing ethylenically unsaturated monomers are based on metallocenes. Metallocenes can generally be characterized as coordination compounds incorporating one or more cyclopentadienyl (Cp) groups (which may be substituted or unsubstituted) coordinated to transition metals via π bonds. Highly active polymerization catalysts are formed when certain metallocene compounds are combined with activators or cocatalysts such as methylaluminoxane (MAO) and possibly also alkylating / scavenging agents such as trialkylaluminum compounds . Various types of metallocenes are known in the art. For example, as described in U.S. Patent No. 5,324,800...

Claims

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Application Information

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IPC IPC(8): C08F4/645C08F4/642C08F4/646C08F4/659C08F4/6592C08F10/00C08F110/06
CPCC08F4/65904C08F4/65912C08F4/65927C08F10/00C08F110/06C08F4/65916C08F2500/16C08F2500/18C08F2500/12C08F2500/03C08F2500/15C08F4/642
Inventor W·J·高瑟M·洛佩斯D·J·劳舍尔D·G·小坎贝尔M·E·克尔
Owner FINA TECH
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