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Olefin polymerization method

An olefin polymerization and olefin technology, applied in the field of olefin polymerization, can solve the problems of low catalytic activity and low efficiency, and achieve the effect of stable mesoporous structure

Active Publication Date: 2013-09-25
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 low catalytic activity of the supported metallocene catalysts in the prior art, resulting in the low efficiency of the olefin polymerization reaction using the supported metallocene catalyst, and to provide a high-efficiency olefin polymerization method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0064] Mix 1.5 grams of CTAB (cetyltrimethylammonium bromide), 1.5 mL of polyethylene glycol octylphenyl ether (Triton-X100) with 29.6 grams of concentrated hydrochloric acid (37% by weight) Contact with a hydrochloric acid solution of 75 grams of water, stir at 40°C until CTAB is completely dissolved, add 4.35 grams of tetraethyl orthosilicate to the above solution, stir at 40°C for 15 minutes, and stand at 40°C for 24 hours, After filtering, washing and drying, calcining at 600°C for 24 hours, the carrier JKQ was obtained;

[0065] Under nitrogen protection, JKQ was calcined at 400°C for 10 hours to remove hydroxyl groups and residual moisture, thereby obtaining thermally activated JKQ;

[0066] 0.3407 g of activated JKQ was transferred to a 250 ml glass reactor fully replaced by nitrogen, and 20 ml of refined toluene (refluxing via sodium for 24 hours) and 0.4 g of methylalumoxane (purchased from Albemarle, USA) were added , and stirred at 50 °C for 4 hours. After the rea...

Embodiment 1

[0078] This example serves to illustrate the olefin polymerization process according to the present invention.

[0079] 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 1 mole / liter of triethylaluminum (TEA, purchased from Zhejiang Furuide Chemical Co., Ltd.) hexane solution, then add 43.3 mg of JKQ-BU, feed ethylene to raise the pressure to 1.0MPa and maintain it at 1.0MPa, React at 70°C for 1 hour. Obtain 213 grams of polyethylene particle powder, the bulk density (BD) of this polyethylene particle powder is 0.306g / ml, melt index MI 2.16 = 0.026 g / 10 min. It was determined by calculation that the efficiency of the catalyst was 4919g PE / gcat h (ie, 1.1×10 9 g PE / (mol Zr h)).

Embodiment 2

[0081] This example serves to illustrate the olefin polymerization process according to the present invention.

[0082] 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 1 mole / liter triethylaluminum (TEA) hexane solution and 10 milliliters of hexene, then add 40.3 milligrams of JKQ-BU, feed ethylene to raise the pressure to 1.0 MPa and maintain it at 1.0 MPa, react at 70 ° C for 1 Hour. 269 ​​grams of polymer were obtained with a bulk density (BD) of 0.321 g / ml and a melt index MI 2.16 = 0.384 g / 10 min. It is determined by calculation that the efficiency of the catalyst is 6675g PE / gcat h (ie, 1.5×10 9 g PE / (mol Zr h)).

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Abstract

The invention provides an olefin polymerization method, which comprises the following steps that: under an olefin polymerization condition, at least one kind of olefin is contacted with a load type metallocene catalyst. The olefin polymerization method is characterized in that the load type metallocene catalyst 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 in the formula 1. According to the olefin polymerization method provided by the invention, the activity of the load type metallocene catalyst for catalyzing cinyl polymerization is 1.5*109gPE / (mol Zr h), while the activity of active components with the same load of 955 silica gel generally used in industry is only 5.1*107gPE / (mol Zr h).

Description

technical field [0001] The present invention relates to a method for polymerizing olefins. 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 a highly efficient 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 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 is to load the soluble metallocene catalyst. At present, there are many research reports on metallocene loading, among which SiO 2 Such as silica gel 955 is the mos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/00C08F36/02C08F110/02C08F210/16C08F4/6592C08F4/02
Inventor 邱波谢伦嘉亢宇王洪涛王彦强郭顺郑刚刘长城
Owner CHINA PETROLEUM & CHEM CORP
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