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Application of metallocene catalyst-loaded hexagonal mesoporous material to olefinic polymerization

A mesoporous material, ethylene polymerization technology, applied in the field of olefin polymerization, can solve the problems of low ethylene polymerization activity, poor thermal and hydrothermal stability, collapse of pore walls, etc.

Active Publication Date: 2013-06-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main reason for the low ethylene polymerization activity of the mesoporous material MCM-41 after loading the catalyst is that the thermal and hydrothermal stability of the pore wall structure of MCM-41 is poor, and the pore wall partially collapses during the loading process, which affects the loading. effect, so that it affects the catalytic activity

Method used

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  • Application of metallocene catalyst-loaded hexagonal mesoporous material to olefinic polymerization
  • Application of metallocene catalyst-loaded hexagonal mesoporous material to olefinic polymerization
  • Application of metallocene catalyst-loaded hexagonal mesoporous material to olefinic polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Preparation of hexagonal mesoporous materials supporting cocatalyst methylaluminoxane (MAO) and metallocene catalyst precursor bis(1-methyl-3-butyl-cyclopentadienyl)zirconium dichloride:

[0035] (1) 2.0 grams of F108 (Fuka company trade name Substance F108) with 5.24 g K 2 SO 4 Add to 60 grams of 2N (2N) hydrochloric acid solution, stir at 38°C until F108 is completely dissolved;

[0036] (2) Add 4.2 grams of ethyl orthosilicate to the above solution, stir at 38°C for 15 minutes, and stand at 38°C for 24 hours;

[0037] (3) Obtain the original powder mesoporous material after adding 100 grams of deionized water for dilution, filtering, washing and drying;

[0038] (4) Calcining the original powder mesoporous material at 400°C for 10 hours to remove the template agent to obtain the hexagonal mesoporous material;

[0039] (5) Calcining the hexagonal mesoporous material at 400°C for 10 hours under the protection of nitrogen (thermal activation), removing the hydroxyl...

Embodiment 2

[0043] Preparation of hexagonal mesoporous materials supporting cocatalyst methylaluminoxane (MAO) and metallocene catalyst precursor bis(n-butylcyclopentadienyl)zirconium dichloride BUCP:

[0044] The steps for preparing the cocatalyst-supported methylaluminoxane / FDU6 complex carrier (MAO / FDU6) are the same as in Example 1. Preparation of hexagonal mesoporous materials supporting metallocene catalyst precursor bis(n-butylcyclopentadienyl)zirconium dichloride BUCP:

[0045] Under the protection of nitrogen, add the methylaluminoxane / FDU6 complex carrier into the reactor, add 20 ml of refined toluene, stir to form a slurry, and slowly add 43 mg of the metallocene catalyst precursor dropwise at 30°C Bis(n-butylcyclopentadienyl)zirconium dichloride) BUCP, stirred for 0.5 hours. After the reaction was finished, let stand, filter the liquid, wash three times with 20 milliliters of toluene, then wash twice with 40 milliliters of hexane, dry the solid with nitrogen to obtain a catal...

Embodiment 3

[0047] FDU6-MB Ethylene Homopolymerization

[0048] In a 2-liter stainless steel autoclave, replace three times with nitrogen and ethylene respectively, then add 200 milliliters of hexane solvent, raise the temperature of the kettle to 80 ° C, then add the remaining 800 milliliters of hexane solvent, with the addition of hexane, Add 2 ml of triethylaluminum (TEA) hexane solution with a concentration of 1 mol / L, and then add 157.6 mg of FDU6-MB, raise and maintain the pressure to 1.0 MPa, and react at 80° C. for 1 hour. After the end of the polymerization reaction, the polyethylene particle powder was collected and weighed to obtain 311 grams. The efficiency of the catalyst was 1973g PE / gcat h (1.7 × 10 8 gPE / (mol Zr h)), bulk density (BD) is 0.34g / ml, melt index: MI 2.16 =0.017g / 10min.

[0049] FDU6-MB Ethylene Copolymerization

[0050] In a 2-liter stainless steel autoclave, replace three times with nitrogen and ethylene respectively, then add 200 milliliters of hexane sol...

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Abstract

The invention relates to application of a metallocene catalyst-loaded hexagonal mesoporous material to olefinic polymerization. The hexagonal mesoporous material is a hexagonal mesoporous material with the particle size of between 3 and 20 microns. The outer surface and / or inner pore wall of the hexagonal mesoporous material is loaded with methylaluminoxane (MAO) serving as a cocatalyst and a metallocene catalyst precursor. After the hexagonal mesoporous material is loaded, the mesoporous structure is stable, a microstructure is still a hexagon with high dispersibility and is similar to the microstructure of industrial common silica gel, and olefinic polymerization activity is remarkably higher than that of MCM-41; and compared with the bar-shaped structure of the MCM-41, the structure ofthe hexagonal mesoporous material is more beneficial to industrial application.

Description

technical field [0001] The invention relates to the application of metallocene-loaded hexagonal mesoporous materials in polyolefin reaction, belonging to the field of olefin polymerization. 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. (Angew.Chem., 1980,19,390; Adv. .Organoment.Chem., 1980, 18, 99.) developed a high-efficiency cocatalyst methylaluminoxane (MAO), making the research on metallocene catalysts enter 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 particle shape, it cannot be used in the widely used slurry method or gas phase polymerization process, an effective solution to the above problems The way i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/02C08F4/02C08F4/6592
Inventor 邱波谢伦嘉亢宇王彦强周歆郑刚赵思源邓晓音刘长城
Owner CHINA PETROLEUM & CHEM CORP
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