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Loaded metallocene catalyst and preparation method thereof

A technology of metallocene catalysts and metallocene compounds, applied in the field of supported metallocene catalysts and their preparation, can solve the problems of small particle size and low catalytic activity of mesoporous materials, and achieve the effect of ensuring particle size and catalytic activity

Active Publication Date: 2014-04-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The object of the present invention is to overcome the problems that the catalytic activity of the supported metallocene silica gel catalyst in the prior art is still low and the particle size of the mesoporous material is small, and provide a high-activity large-particle supported metallocene catalyst

Method used

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  • Loaded metallocene catalyst and preparation method thereof
  • Loaded metallocene catalyst and preparation method thereof
  • Loaded metallocene catalyst and preparation method thereof

Examples

Experimental program
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Embodiment approach

[0059] According to one embodiment of the present invention, the preparation method of described supported metallocene catalyst comprises the following steps:

[0060] In the first step, the three-block copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene and N,N-dimethylformamide (DMF) are added to aqueous hydrochloric acid, and the molar feed ratio is

[0061] Tri-block copolymer polyethylene oxide-polyoxypropylene-polyoxyethylene: N, N-dimethylformamide (DMF): water: hydrogen chloride = 1: 300-700: 10000-20000: 100-500, preferably 1:550-650:10000-13000:150-480, especially preferably 1:596:11411:326,

[0062] Stir at 25-60°C until dissolved;

[0063] In the second step, add ethyl orthosilicate to the solution obtained in the previous step, stir at 25-60°C for 1-2 hours, then add silica gel, and stir for another 10-40 hours; the mixture of ethyl orthosilicate and silica gel The weight ratio may be 3-6:1, preferably 4-5:1, more preferably 4.45:1.

[0064] Step 3, filt...

preparation example 1

[0076] This preparation example is used to illustrate the supported metallocene catalyst and its preparation method according to the present invention.

[0077] Add 2.0 grams of P123 and 15 grams of N,N-dimethylformamide (DMF) and 64ml of water into 11.2 grams of 37% hydrochloric acid solution, stir at 40°C until P123 is completely dissolved; then add 4.45 grams of ethyl orthosilicate Add the ester to the above solution and stir at 40°C for 1 hour, then add 1 gram of industrial ES955 silica gel, filter, wash, and dry to obtain the original powder composite material; calcinate the composite material in a muffle furnace at 600°C for 24 hours, remove Templating agent to obtain spherical mesoporous silica (named GJ-MBQ) as the final product.

[0078] The above composite material GJ-MBQ was calcined at 400°C for 10 hours under the protection of nitrogen to remove hydroxyl groups and residual moisture, thereby obtaining a thermally activated composite material.

[0079] Transfer 0....

Embodiment 1

[0091] This example is used to illustrate the catalytic activity of the supported metallocene catalyst according to the present invention.

[0092] In a 2-liter stainless steel autoclave, replace three times each with nitrogen and ethylene, then add 200 ml of hexane, raise the temperature of the kettle to 80 ° C, then add 800 ml of hexane, and add 2 ml of hexane with the addition of hexane The concentration is 1 mole / liter triethylaluminum (TEA) hexane solution, then add 60.6 mg MAO / GJ-MBQ-BU, feed ethylene to raise the pressure to 1.0MPa and maintain it at 1.0MPa, and react at 70°C 1 hour. Obtain 146 grams of polyethylene particle powder, the bulk density (BD) of this polyethylene particle powder is 0.317g / ml, melt index MI 2.16 = 0.051 g / 10 min. It is determined by calculation that the efficiency of the catalyst is 2409g PE / gcat h (ie, 6.2×10 7 g PE / (mol Zr h)).

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Abstract

The invention provides a loaded metallocene catalyst and a preparation method thereof. The catalyst comprises a carrier and a metallocene compound and alkyl aluminoxane which are loaded on the carrier, wherein the carrier is rodlike macroporous silica, the average particle diameter of the carrier is 20-80 micrometers, the specific surface area is 400-700 m<2> / g, the pore volume is 0.3-1.5 ml / g, the most probable aperture is 3-20 nanometers; the metallocene compound has the structure shown in formula 1, wherein M is one of titanium, zirconium and hafnium, and X is halogen. When the loaded metallocene catalyst is used for catalyzing olefin to polymerize, the catalytic efficiency can reach 2409 g PE / gcat-h.

Description

technical field [0001] The invention relates to a supported metallocene catalyst and a preparation method thereof. Background technique [0002] The development and application of metallocene catalysts is another major breakthrough in the field of olefin polymerization catalysts after the traditional Ziegler-Natta catalysts. Due to the large amount of methylaluminoxane (MAO) required to achieve high activity of homogeneous metallocene catalysts, the production cost is high, and the obtained polymer has no particle shape, it cannot be used in the widely used slurry method or gas phase polymerization process. use. Moreover, the activity of the metallocene catalyst is very high, and it is prone to localized polymerization at a faster rate during the polymerization reaction, which in turn leads to detonation. [0003] An effective way to solve the above problems is to carry out loading treatment on soluble metallocene catalysts. At present, there are many reports on the suppo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/6592C08F4/02C08F10/00
Inventor 亢宇谢伦嘉邱波郭顺王洪涛张明森刘长城张伟杨菁梁中伟
Owner CHINA PETROLEUM & CHEM CORP
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