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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: 2012-10-10
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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Effect test

Embodiment approach

[0059] According to an embodiment of the present invention, the preparation method of the supported metallocene catalyst includes the following steps:

[0060] In the first step, add the triblock copolymer polyoxyethylene-polyoxypropylene-polyoxyethylene and N,N-dimethylformamide (DMF) to the hydrochloric acid aqueous solution at a molar ratio of

[0061] The triblock copolymer polyethylene oxide-polypropylene oxide-polyethylene oxide: N, N-dimethylformamide (DMF): water: hydrogen chloride=1: 300-700: 10000-20000: 100-500, preferably 1:550-650:10000-13000:150-480, particularly preferably 1:596:1411:326,

[0062] Stir to dissolve at 25-60℃;

[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 10-40 hours; The weight ratio may be 3-6:1, preferably 4-5:1, more preferably 4.45:1.

[0064] In the third step, the crystallization product is filtered, washed, and dried to obtain the...

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 g of P123, 15 g of N, N-dimethylformamide (DMF) and 64 ml of water to 11.2 g of 37% hydrochloric acid solution, and stir at 40°C until P123 is completely dissolved; then 4.45 g of ethyl orthosilicate The ester was added to the above solution and stirred at 40°C for 1 hour, and then 1 gram of industrial ES955 silica gel was added. After filtering, washing and drying, the raw powder composite material was obtained; the composite material was calcined in a muffle furnace at 600°C for 24 hours to remove Template agent to obtain the final product of spherical mesoporous silica (named GJ-MBQ).

[0078] The above-mentioned composite material GJ-MBQ is 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.

...

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 with nitrogen and ethylene three times each, then add 200 ml of hexane, raise the temperature of the kettle to 80°C, and then add 800 ml of hexane, and with the addition of hexane, add 2 ml A triethylaluminum (TEA) hexane solution with a concentration of 1 mol / L, then 60.6 mg MAO / GJ-MBQ-BU was added, and ethylene was introduced to increase the pressure to 1.0 MPa and maintain it at 1.0 MPa, and react at 70°C 1 hour. Obtained 146 grams of polyethylene particle powder, the bulk density (BD) of the polyethylene particle powder is 0.317g / ml, and the melt index MI 2.16 =0.051g / 10min. After calculation, the efficiency of the catalyst is 2409g PE / gcat·h (that is, 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 for the homogeneous metallocene catalyst to achieve high activity, the production cost is high, and the obtained polymer has no particle shape, which cannot be used in widely used slurry or gas phase polymerization processes. use. In addition, the metallocene catalyst has high activity and is prone to local polymerization speed during the polymerization reaction, which leads to explosion. [0003] The effective way to solve the above-mentioned problems is to support the soluble metallocene catalyst. At present, there are many reports on the support of metallocene catalysts, among which SiO 2 As the ...

Claims

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Application Information

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Patent Type & Authority Applications(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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