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Load type metallocene catalyst as well as preparation method and application thereof

A technology of metallocene catalyst and metallocene compound, applied in the field of catalyst science, can solve the problems such as difficult to support catalyst, consumption of MAO, complicated preparation, etc., and achieve the effect of overcoming sticking kettle phenomenon, simple preparation and high catalytic activity

Inactive Publication Date: 2010-11-10
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In Chinese patent CN135877A, zirconocene dichloride, zirconium diindene dichloride and bis(n-butylcyclopentadienyl) zirconium dichloride are supported on magnesium chloride, and organic crosslinking agents such as polyols are added during the preparation process to prepare the Loaded metallocene catalyst consumes a lot of MAO, and the preparation is cumbersome
This method is too complicated, and it is not easy to load a large amount of catalyst

Method used

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  • Load type metallocene catalyst as well as preparation method and application thereof
  • Load type metallocene catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A preparation method of supported metallocene catalyst, comprising the following steps:

[0032] (1) Preparation of ligand: 1-bromo-5-(4-methylphenoxy)pentane [p-CH 3 C 6 h 4 O(CH 2 ) 5 Br]

[0033] Under an ice-water bath, 10.8 g (0.1 mol) of p-cresol was added to 100 mL of methanol solution containing 4.4 g (0.1 mol) of sodium hydroxide, and stirred for 30 minutes to obtain a reddish methanol solution of sodium p-cresate. Under stirring, the solution was added dropwise to 1.0 mol α, ω-dibromopentane, heated to reflux, and the gas phase followed the reaction for about 5 hours. After the reaction, the solvent methanol was recovered by atmospheric distillation, the residual liquid was cooled to room temperature, 30 mL of distilled water was added, the liquid was separated, the organic phase was washed twice with 20 mL of distilled water, dried with anhydrous magnesium sulfate, the solvent and raw materials were recovered by rotary evaporation, and 123 -126°C (2mmHg...

Embodiment 2

[0040] A preparation method of supported metallocene catalyst, comprising the following steps:

[0041] (1) Preparation of ligand: same as Example 1;

[0042] (2) Preparation of main catalyst: heteroatom metallocene compound [p-CH 3 C 6 h 4 O(CH 2 ) 5 Ind] 2 ZrCl 2 (B)

[0043] The preparation method is the same as in Example 1, except that the sodium cyclopentadiene is changed to indenyllithium to obtain 1.69g of complex B with a yield of 51.2%. 42 h 46 Cl 2 o 2 Zr: Calculated: C, 67.72%, H, 6.22%, found, C, 67.65%, H, 6.31%.

[0044] (3) Supported metallocene catalyst S-B catalyzes ethylene polymerization

[0045] Take 3.0 mg of the main catalyst B prepared in step (2) and dissolve it in 10 mL of dry toluene, then slowly add 1.5 mol / L of 1 mL of methylaluminoxane toluene solution, after the addition is completed, react at 40 ° C for 2 h, and then add to In the toluene suspension containing 0.03g dry clay, stir and mix for 0.5h. Then add the mixed solution into ...

Embodiment 4

[0054] (1) Preparation of ligand: same as Example 3;

[0055] Heteroatom metallocene compounds [p-CH 3 C 6 h 4 O(CH 2 ) 6 Ind] 2 ZrCl 2 (D)

[0056] (2) Preparation of main catalyst: preparation method is the same as embodiment 1 step (2), adopting the 1-bromo-6-(4-methylphenoxy) hexane that step (1) makes in embodiment 3 is raw material , changing the cyclopentadienyl sodium into indenyl lithium to obtain 2.04g of complex C with a yield of 56.1%, C 44 h 50 Cl 2 o 2 Zr: Calculated: C, 68.37%, H, 6.52%, found, C, 68.25%, H, 6.61%.

[0057] (3) Supported metallocene catalyst S-D catalyzed ethylene polymerization

[0058] Dissolve 6 mg of complex D in 10 mL of dry toluene, then slowly add 1.5 mol / L of 1 mL of methylalumoxane toluene solution, after the addition is complete, react at 40°C for 2 h, then add to toluene containing 0.05 g of dry clay to suspend solution, stirred and mixed for 0.5h. Then add the mixed solution into a 2L high-pressure stainless steel stirr...

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Abstract

The invention relates to a load type metallocene catalyst as well as a preparation method and application thereof. The catalyst comprises a main catalyst, an auxiliary catalyst and a carrier, wherein the main catalyst and the auxiliary catalyst are loaded on the carrier, and thus, the load type metallocene catalyst is formed. The catalyst is applied to the polymerization of an olefin monomer. Compared with the prior art, the load type metallocene catalyst has the advantages of simple preparation and higher catalytic activity; and in the presence of phenoxyl, a metallocene compound can be completely loaded on clay so that the load type metallocene catalyst does not drop in the process of polymerization, thereby overcoming the phenomenon of sticking kettles.

Description

technical field [0001] The invention belongs to the field of catalyst science and technology, and relates to a supported metallocene catalyst and its preparation method and application. Background technique [0002] In the field of polyolefin industry, metallocene catalyst is another technological leap after Zieglar-natta catalyst, which opens up a new field of polyolefin materials and provides the possibility for customized development of new polyolefins. For example: Zieglar-Natta catalysts can only produce isotactic polypropylene, while using metallocenes can directionally prepare various polypropylenes: isotactic polypropylene, syndiotactic polypropylene, atactic polypropylene and Semi-isotactic polypropylene. In short, the use of metallocenes to prepare polyolefins can control the conformation of the polymer as well as the physical properties of the polymer. [0003] Homogeneous metallocene catalyst olefin polymerization technology has very large limitations, such as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/00C08F4/6592C08F2/14C08F2/34C08F10/02C08F10/06
Inventor 王临才秦一秀吴向阳徐静安唐毅平
Owner SHANGHAI RES INST OF CHEM IND
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