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Supported metallocene catalyst and preparation method thereof

A metallocene catalyst and metallocene compound technology are applied in the field of supported metallocene catalysts and their preparation, which can solve the problems of high cost and low mechanical strength of mesoporous materials, and achieve the effects 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

[0015] The purpose of the present invention is to overcome the problems of high cost of supported metallocene catalysts and low mechanical strength of mesoporous materials in the prior art, and provide a high-performance catalyst with low cost, stable structure, good performance and mechanical strength. Specific Surface Area Supported Metallocene Catalysts

Method used

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  • Supported metallocene catalyst and preparation method thereof
  • Supported metallocene catalyst and preparation method thereof
  • Supported metallocene catalyst and preparation method thereof

Examples

Experimental program
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Embodiment approach

[0063] According to one embodiment of the present invention, the preparation method of described supported metallocene catalyst comprises the following steps:

[0064] In the first step, polyethylene glycol octyl phenyl ether (triton X-100) and cetyltrimethylammonium bromide (CTAB) are added to aqueous hydrochloric acid, and the molar charge ratio is

[0065] Sodium silicate: polyethylene glycol octylphenyl ether (Triton X-100): cetyltrimethylammonium bromide (CTAB): hydrogen chloride: water = 1: 0.01-0.5: 0.1-0.6: 5-50:100-500, preferably 1:0.01-0.3:0.1-0.4:5-20:100-300, particularly preferably 1:0.03:0.11:7.97:111,

[0066] Stir at 25-60°C until dissolved;

[0067] Step 2, add sodium silicate to the solution obtained in the previous step and stir at 25-60°C for 10-40 minutes until dissolved;

[0068] Step 3: crystallize the product obtained in the previous step for 10-40 hours at a temperature of 25-60°C, filter, wash, and dry the crystallized product to obtain a spherical...

preparation example 1

[0079] This preparation example is used to illustrate the supported metallocene catalyst and its preparation method according to the present invention.

[0080] 1.5 grams of cetyltrimethylammonium bromide (CTAB) and 1.5 ml of polyethylene glycol octylphenyl ether (Triton X-100) with a density of 1.07 g / ml and a concentration of 5% by weight were added In the hydrochloric acid solution that is the concentrated hydrochloric acid of 37% by weight and 75 grams of water by 29.6 gram concentration, stir until CTAB and Triton X-100 dissolve completely at 40 ℃; The solution was stirred at 40°C for 15 minutes, the sodium silicate was completely dissolved, and then crystallized at 40°C for 24 hours. After filtering, washing and drying, the original powder mesoporous material was obtained; the original powder mesoporous material was placed in a muffle furnace for 600 ℃ for 24 hours to remove the template agent and obtain a spherical mesoporous silica material (named JKQ).

[0081] The a...

Embodiment 1

[0094] This example is used to illustrate the catalytic activity of the supported metallocene catalyst according to the present invention.

[0095] 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 of triethylaluminum (TEA) hexane solution, then add 49.9 mg of JKQ-BU, feed ethylene to raise the pressure to 1.0 MPa and maintain it at 1.0 MPa, and react at 70°C for 1 hour. Obtain 91 grams of polyethylene particle powder, the bulk density (BD) of this polyethylene particle powder is 0.304g / ml, melt index MI 2.16 = 0.005 g / 10 min. It was determined by calculation that the efficiency of the catalyst was 1824g PE / gcat h (ie, 4.2×10 7 g PE / (mol Zrh)).

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Abstract

The invention provides a supported metallocene catalyst and its preparation method, and is characterized in that the catalyst comprises a carrier and a metallocene compound and alkyl aluminoxane which are loaded on the carrier. The carrier is spherical mesoporous silicon dioxide. The average particle diameter of the carrier is 1-10 micrometers, its specific surface area is 1000-2000 square meter / gram, its pore volume is 0.3-1.5 ml / g, and its most probable pore size is 4-20 nanometers. The metallocene compound has a structure as shown in the formula 1, wherein M is one selected from the group consisting of titanium, zirconium and hafnium and X is halogen. When the supported metallocene catalyst provided by the invention is used to catalyze alkene polymerization, the catalytic efficiency can reach 1909 g PE / gcath.

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 亢宇张明森王洪涛邱波郭顺刘长城
Owner CHINA PETROLEUM & CHEM CORP
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