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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 low catalytic activity and achieve the effects of high catalytic activity, high catalytic activity and stable structure

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

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Problems solved by technology

[0016] The purpose of the present invention is to overcome the problem that the catalytic activity of the supported metallocene catalyst of the prior art is still low, and a kind of highly active supported metallocene catalyst is provided

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

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preparation example Construction

[0045] According to the preparation method of the present invention, the types of the carrier, the alkylaluminoxane and the metallocene compound have been described above, and will not be repeated here.

[0046] The method for loading the alkylaluminoxane and the metallocene compound on the carrier may be various loading methods known in the art, such as dipping and spraying. The method of impregnation can make the solution more fully enter the pores on the carrier, so impregnation is preferred in the present invention.

[0047] The method for preparing the above-mentioned supported metallocene catalyst of the present invention further comprises heating the carrier at a temperature of 300-500°C for 5-20 hours under the protection of an inert gas before loading the alkylaluminoxane .

[0048] The method for preparing the above-mentioned supported metallocene catalyst of the present invention, for example: may comprise the following steps:

[0049] (1) Thermal activation step,...

Embodiment 1

[0057] This example is used to illustrate the supported metallocene catalyst and its preparation method according to the present invention.

[0058] 1) The rod-shaped mesoporous material SBA-15 (commercially purchased from Changchun Jilin University High-tech Co., Ltd., the length of the rod is 30-100 microns, and its pore structure parameters are shown in Table 1) was calcined at 400 ° C for 10 hour (thermal activation), remove hydroxyl group and residual moisture, obtain the rod-shaped mesoporous material after thermal activation;

[0059]2) Transfer 0.4 g of the thermally activated rod-shaped mesoporous material to a 250 ml glass reactor fully replaced by nitrogen, add 10 ml of refined toluene, methyl aluminoxane (MAO, commercially available from Albemarle, USA) 0.47 g of auxiliary agent was stirred at 50° C. for 4 hours. After completion, wash three times with 20 ml of hexane, and finally dry the solid with nitrogen to obtain a methylaluminoxane / SBA-15 complex carrier (MA...

experiment Embodiment 1

[0070] This experimental example is used to illustrate the catalytic activity of the supported catalyst according to the present invention.

[0071] In a 2-liter stainless steel autoclave, replace three times with nitrogen and ethylene, then add 200 milliliters of hexane solvent, raise the temperature of the kettle to 80 ° C, and then add 800 milliliters of hexane solvent. With the addition of hexane, the 2 ml of 1 mol / L triethylaluminum (TEA) hexane solution was added, followed by 65.5 mg of SBA-15-BU-1, ethylene was introduced to raise and maintain the pressure to 1.0 MPa, and the reaction was carried out at 70°C for 1 hour. After the end of the polymerization reaction, the polyethylene particle powder was collected and weighed to obtain 421 grams. The efficiency of the catalyst was 6427gPE / (gcat h)(8.4×10 7 gPE / (mol Zr h)), the bulk density (BD) of polyethylene is 0.326g / ml, the melt index: MI 2.16 = 0.061 g / 10 min.

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Abstract

The invention provides a loaded metallocene catalyst, which is characterized by comprising a carrier, and a metallocene compound and alkylaluminoxane loaded on the carrier, wherein the carrier is SBA-15; the metallocene catalyst has a structure shown as a formula 1; in the formula 1, R1, R2, R3, R4, R5, R1', R2', R3', R4' and R5' are hydrogen or alkyl with 1-5 carbon atoms respectively and independently; at least one of R1, R2, R3, R4 and R5 is alkyl with 1-5 carbon atoms; at least one of R1', R2', R3', R4' and R5' is the alkyl with 1-5 carbon atoms; M is one of titanium, zirconium and hafnium; and X is halogen. In the loaded metallocene catalyst provided by the invention, the metallocene catalyst has a sandwich structure, and cyclopentadienyl is provided with a substituent. By loading the substituent on a mesoporous material SBA-15 which has high mechanical strength and high catalytic adsorption property, a loaded metallocene catalyst with a stable structure and high catalytic activity can be obtained, so that the loaded metallocene catalyst has high catalytic activity.

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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IPC IPC(8): C08F10/00C08F110/02C08F210/02C08F4/6592C08F4/02
Inventor 亢宇谢伦嘉邱波王洪涛王彦强郭顺郑刚刘长城周歆王伟邓晓音王红英赵思源姜健准
Owner CHINA PETROLEUM & CHEM CORP
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