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Load type metallocene catalyst and preparation method thereof

A technology of metallocene catalyst and metallocene compound, which is applied in the field of supported metallocene catalyst and its preparation, and can solve the problem of low ethylene polymerization activity

Active Publication Date: 2012-05-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to overcome the shortcomings of the low activity of supported metallocene catalysts in the prior art for catalyzing ethylene polymerization, and provide a highly active supported metallocene catalyst

Method used

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  • Load type metallocene catalyst and preparation method thereof
  • Load type metallocene catalyst and preparation method thereof
  • Load type metallocene catalyst and preparation method thereof

Examples

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Embodiment approach

[0045] According to another embodiment of the present invention, the spherical mesoporous silica carrier can be prepared by a method comprising the following steps: in the presence of a templating agent, contacting a silicate ester with an acidic aqueous solution, and mixing the resulting mixture Crystallization under crystallization conditions, the resulting crystallization product is heated to remove the template agent, the template agent is hexadecyltrimethylammonium bromide and polyethylene glycol octylphenyl ether (also known as Triton X-100).

[0046] According to the present invention, the molar ratio of the acid in the acidic aqueous solution and the water in the acidic aqueous solution can be within a certain range Change, preferably, the molar ratio of the acid and water in the silicate, cetyltrimethylammonium bromide, polyethylene glycol octylphenyl ether (Triton X-100), acidic aqueous solution 1: 0.1-0.6: 0.1-0.5: 5-50: 100-500, more preferably, the silicate, cety...

Embodiment 1

[0066] This example is used to illustrate the supported metallocene catalyst provided by the present invention and its preparation method.

[0067] 1.5 g of CTAB (hexadecyl trimethyl ammonium bromide), 1.5 mL of polyethylene glycol octyl phenyl ether (Triton-X100, purchased from Shanghai Sangon Bioengineering Co., Ltd., product number TB0198) were mixed with Contact with a hydrochloric acid solution containing 29.6 grams of concentrated hydrochloric acid (concentration of 37% by weight) and 75 grams of water, stirring at 40 ° C until CTAB is completely dissolved, adding 4.35 grams of tetraethyl orthosilicate to the above solution, at 40 ° C. Stir for 15 minutes, stand at 40°C for 24 hours, filter, wash and dry, then calcinate at 600°C for 24 hours to remove the template agent to obtain the carrier JKQ;

[0068] Under nitrogen protection, JKQ was calcined at 400 °C for 10 hours to remove hydroxyl groups and residual moisture, thereby obtaining thermally activated JKQ;

[0069]...

experiment Embodiment 1

[0081] This experimental example is used to illustrate the catalytic activity of the supported metallocene catalyst according to the present invention.

[0082] In a 2-liter stainless steel autoclave, replace three times with nitrogen and ethylene, 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 of hexane 1 mol / L of triethylaluminum (TEA, purchased from Zhejiang Freed Chemical Co., Ltd.) in hexane, followed by adding 43.3 mg of JKQ-BU, and feeding 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 213 grams of polyethylene granular powder, the bulk density (BD) of this polyethylene granular powder is 0.306g / mL, melt index MI 2.16 =0.026g / 10min. It was determined by calculation that the efficiency of the catalyst was 4919 g PE / g cat h (ie, 1.1 × 10 9 g PE / (mol Zr h)).

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Abstract

The invention provides a load type metallocene catalyst, which comprises a carrier, and a metallocene compound and alkylaluminoxane which are on the carrier, wherein the carrier is a spherical mesoporous silicon dioxide carrier, and the metallocene compound has a structure shown by the formula 1, wherein R1, R2, R3, R4, R5, R1', R2', R3', R4'and R5' respectively and independently form alkyl of hydrogen or C1-C5, at least one of R1, R2, R3, R4 and R5 is alkyl of C1-C5, at least one of R1', R2', R3', R4'and R5' is alkyl of C1-C5, M is one of titanium, zirconium and hafnium, and X is halogen. The invention also provides a preparation method of the load type metallocene catalyst. The load type metallocene catalyst provided by the invention has a stable structure and high catalytic activity. The formula 1 is shown in the accompanying drawing.

Description

technical field [0001] The present 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. Especially in the 1980s, Kaminsky and Sinn et al. developed high-efficiency cocatalyst methylaluminoxane (MAO). The research on metallocene catalysts has entered a stage of rapid development. Due to the large amount of MAO required for the homogeneous metallocene catalyst to achieve high activity, the production cost is high, and the obtained polymer has no granular shape, which cannot be used in the widely used slurry method or gas phase polymerization process. The solution is to support the soluble metallocene catalyst. At present, there are many reports on metallocene loading, among which SiO 2 For example, 955 silica gel is the most widely...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F110/02C08F210/02C08F4/6592C08F4/02
Inventor 亢宇谢伦嘉邱波王洪涛王彦强郭顺刘长城赵思源周歆
Owner CHINA PETROLEUM & CHEM CORP
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