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Preparation method of metallocene catalyst

A technology of metallocene catalysts and metallocene compounds, which is applied in the field of preparation of metallocene catalysts and can solve the problems of reducing the aging resistance of polymers

Active Publication Date: 2015-03-25
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A small amount of ethane in the polymerization system has limited influence on the polymerization system, but for long-term continuous polymerization reactions, the continuous generation of ethane will inevitably have a negative impact on the polymerization system; in addition, a molecule of hydrogen generated during the polymerization process will Leaving a double bond on the substance will reduce the aging resistance of the polymer

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0034] In 500 mL of tetrahydrofuran, add 4 g of triisobutylaluminum and 0.5 g of nickel acetylacetonate to react at room temperature for 2 hours, then add 5 g of Davison955 silica (commercially available) from Grace Company to continue the reaction at room temperature for 4 hours, and remove the solvent Store in nitrogen gas for later use.

[0035]20 g of 10% by mass percentage of methylaluminoxane toluene solution and 0.15 g of bis(pentamethylcyclopentadienyl) zirconium dichloride were stirred at 50°C for 2 hours to obtain the catalyst mother liquor,

[0036] Then silica gel was added into the mother liquor, the reaction was continued at -10°C for 4 hours, and the solid powder catalyst was obtained after removing the solvent.

Embodiment 2

[0043] In 500mL of tetrahydrofuran, add 7g of triisobutylaluminum and 1g of cobalt acetylacetonate to react for 1 hour at -10°C, then add 15g of Davison955 silicon dioxide from Grace Company and react at room temperature for 6 hours. After removing the solvent, seal the obtained silica gel with nitrogen until use.

[0044] 10 g of 10% by mass percentage of methylaluminoxane toluene solution and 0.05 g of bis(tert-butylcyclopentadienyl) zirconium dichloride were stirred at 70° C. for 4 hours to obtain the catalyst mother liquor,

[0045] Then silica gel was added to the mother liquor, the reaction was continued at -10°C for 6 hours, and the solid powder catalyst was obtained after removing the solvent.

Embodiment 3

[0047] In 500mL of tetrahydrofuran, add 1g of triisobutylaluminum and 0.25g of nickel acetylacetonate to react at 50°C for 3 hours, then add 23g of Davison955 silicon dioxide from Grace Company at 50°C for 4 hours, remove the solvent and seal the obtained silica gel with nitrogen stand-by.

[0048] 100 g of 10% by mass percentage of methylaluminoxane toluene solution and 8 g of bis(n-butylcyclopentadienyl) zirconium dichloride were stirred at 50° C. for 2 hours to obtain the catalyst mother liquor,

[0049] Then silica gel was added into the mother liquor, the reaction was continued at -10°C for 4 hours, and the solid powder catalyst was obtained after removing the solvent.

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Abstract

The invention discloses a preparation method of a metallocene catalyst. The method includes preparation of a catalyst mother liquor through reaction of a metallocene compound and a cocatalyst, and carrier loading. The method is characterized in that the carrier before loading is activated by alkyl aluminum and a group VIII metal organic compound, the molar ratio of alkyl aluminum to group VIII metal organic compound n (Al) / n (M1) ranges from 0.1 to 300, M1 represents group VIII metal, the group VIII metal organic compound is preferably at least one acetylacetonate metal compound or naphthenate compound of nickel, palladium, platinum, iron and cobalt. According to the preparation method provided by the invention, the a specific group VIII metal organic compound is introduced into the catalyst to not only reduce the hydrogen produced in the polymerization process but also obviously reduce the number of double bonds in the polymer, so as to obtain a high molecular weight polymer with improved aging resistant performance. The catalyst is applicable to homopolymerization or copolymerization process of various alkenes.

Description

technical field [0001] The invention relates to a preparation method of a metallocene catalyst, in particular to a preparation method of a metallocene catalyst for producing high molecular weight polyolefin. Background technique [0002] Metallocene catalysts are a new generation of olefin polymerization catalysts after Ziegler-Natta catalysts. Compared with Ziegler-Natta catalysts, metallocene catalysts have a single active center and the polymer chain length and comonomer content produced by each active center are almost the same; the catalyst structure is controllable, and the polyolefin molecular chain can be tailored; the catalyst It has high catalytic activity and good hydrogen adjustment sensitivity. Compared with Ziegler-Natta catalyst, polyolefin products with the same fluidity can be obtained under the condition of extremely low hydrogen concentration. [0003] However, it has been found through research that the metallocene catalyst after the catalyst is alkylate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/00C08F110/02C08F4/70
Inventor 张鹏李丽韦少义朱博超王海张平生乔彤森王丹丹李朋朋李广全王雄刘文霞刘强郝萍刘小燕
Owner PETROCHINA CO LTD
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