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A kind of loading method of metallocene catalyst

A metallocene catalyst and negative pressure technology, applied in the field of metallocene catalyst loading, can solve the problems of long loading time and low loading rate, and achieve the effects of improving polymer morphology, shortening preparation time, and being simple and easy to implement.

Inactive Publication Date: 2011-12-21
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

WO97 / 26285 discloses a method for preparing a supported catalyst using a closed reactor under high pressure and high temperature conditions of 5-500 psig. The loading time of the method is long and the loading rate is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1) Take 6.0g of dried and processed specific surface is 305m 2 / g, the pore volume is 1.65cm 3 / g, with an average particle size of 45.3 μm, the silica gel carrier was put into a sealed reaction flask, and the interior of the reaction flask was replaced with nitrogen three times; vacuum was continuously evacuated for 15 minutes under (-0.085) MPa; 50ml12 was added to the flask by starting stirring % of the toluene solution of methylaluminoxane, keep the pressure (-0.065) MPa, and react at 20°C for 0.5 hours;

[0018] 2) Put 16ml of 12% methylaluminoxane toluene solution into another replaced flask, add 0.56g of diindenyl zirconium dichloride, start stirring to dissolve all the diindenyl zirconium dichloride;

[0019] 3) Add the dissolved bisindenyl zirconium dichloride / methylaluminoxane toluene solution into the silica gel, flush with nitrogen to keep the reaction flask under normal pressure, and react at 20°C for 0.5 hours;

[0020] 4) Wash with toluene for 3 times, ...

Embodiment 2

[0028] The reaction conditions are the same as in Example 1, except that 0.56 g of diindenyl zirconium dichloride is replaced by 0.76 g of (indenyl)(cyclopentadienyl) zirconium dichloride.

Embodiment 3

[0030] Reaction condition is the same as embodiment 1, and difference is only to replace 0.56g diindenyl zirconium dichloride with 0.76g two (butyl) (cyclopentadienyl) zirconium dichlorides, the reaction of the first step and the third step The temperature was lowered from 20°C to 5°C.

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PUM

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Abstract

The invention relates to a loading method of a metallocene catalyst. In different stages of catalyst preparation in a closed reaction system, a certain negative pressure is formed in the system, namely: 1) the relative vacuum degree of the inorganic carrier pretreatment step system is ( -0.1)~(-0.075)MPa; 2) The relative vacuum of the system is (-0.065)~(-0.075)MPa when aluminoxane is added to the inorganic carrier; 3) Aluminoxane and metallocene compounds are added to the inorganic carrier After the system returns to normal pressure, each component can enter the pores of the inorganic carrier uniformly and quickly, the loading effect of the catalyst and the polymerization activity are greatly improved, and the polymer morphology is obviously improved. This method is simple and easy to implement, and can greatly improve the The preparation time of the metallocene catalyst is shortened, and the preparation efficiency of the supported catalyst is improved.

Description

technical field [0001] The invention relates to a loading method of a metallocene catalyst. . Background technique [0002] Homogeneous metallocene catalysts have poor polymer morphology for olefin polymerization. Therefore, metallocene catalysts generally need to support metallocenes and other active components on inorganic supports such as SiO2 through a loading method. In order to meet the needs of more polymerization processes, such as gas phase polymerization and slurry polymerization, improve the morphology of polymers, increase catalyst activity and apparent density of polymers, improve the loading effect of active components as much as possible, and increase the stability of active centers Sex is very important. At present, the loading of loaded metallocene catalysts usually firstly handles the carrier, and then loads the metallocene (such as ZL96109534.2, CN02105140.2, ZL03155997.2, US4808561). For better loading effect, CN1307065 provides a Under the action of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/659C08F4/6592C08F4/02C08F10/00
Inventor 曲其昌刘永军仇国贤刘文霞张翠玲韩燕李耀郝萍王海王丹丹韩晓昱姚培洪
Owner PETROCHINA CO LTD
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