Catalyst for ethene polymerization or multipolymer, preparing method thereof

A technology for ethylene polymerization and copolymerization, which is applied in the field of catalysts for ethylene polymerization or copolymerization and its preparation. It can solve the problems of unsatisfactory particle shape of the catalyst, and achieve good particle shape, narrow particle distribution, and good copolymerization performance. Effect

Inactive Publication Date: 2004-12-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Patent CN1229092 improves the preparation method of the catalyst in CN85100997. During the preparation of the catalyst, ethanol is added to modify the magnesium halide, so that the activity of the prepared catalyst in catalyzing ethylene polymerization is greatly improved, but the system still uses the magnesium halide in CN85100997 Therefore, a large amount of titanium tetrahalide is still required for precipitation, and the catalyst still uses a single magnesium dichloride as a carrier, so the particle shape of the catalyst is still not very ideal, and the catalyst particles are easy to break and produce fine polymer powder.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Synthesis of catalyst

[0043] In the reactor fully replaced by high-purity nitrogen, 2.4g of magnesium dichloride, 40ml of toluene treated with molecular sieves, 3.9ml of epichlorohydrin, and 4.1ml of tributyl phosphate were added in sequence, and the temperature was raised to 80°C under stirring. After 2 hours, the solid had completely dissolved to form a homogeneous solution. Add 30ml of dehydrated hexane, 2.3g of silica gel (treated at 600°C for 4 hours, and activated with 0.7mmol of triethylaluminum), cool the system to -25°C, slowly add 8ml of titanium tetrachloride dropwise, and then Slowly raise the temperature to 80°C, react for 2 hours, add 5ml of tetrahydrofuran, and continue the reaction at 80°C for 1 hour. Stop stirring, stand still, the suspension is separated quickly, the supernatant is extracted, washed four times with hexane, and dried with high-purity nitrogen to obtain a solid catalyst with good fluidity and narrow particle size distribution. Th...

Embodiment 2

[0047] (1) The synthesis of catalyst is the same as in Example 1.

[0048] (2) Ethylene slurry polymerization

[0049] A stainless steel reaction kettle with a capacity of 2L, after being fully replaced by high-purity nitrogen, add 1L of hexane, 1.0ml of triethylaluminum with a concentration of 1M, and add 15mg of the catalyst prepared above accurately with a syringe, raise the temperature to 75°C, and inject Hydrogen made the pressure in the kettle reach 0.48Mpa, and then fed ethylene to make the total pressure in the kettle reach 1.03Mpa (gauge pressure), and polymerized at 85°C for 2 hours. The polymerization results are shown in Table 1.

Embodiment 3

[0051] (1) The synthesis of catalyst is the same as in Example 1.

[0052] (2) Gas phase fluidized bed ethylene polymerization

[0053] In the reactor of Φ150 gas-phase fluidized bed, add 350g through the industrial plant base resin DGM-1820 polyethylene powder that dries as base material and 10 grams of triethylaluminum (87mmol). According to the condition, add proportioning to be hydrogen 10.93% (volume ratio), 1-butene 20.43% (volume ratio), ethylene 58.32% (volume ratio), nitrogen 7.02% (volume ratio) mixed gas, make the gas total pressure to 1.7 MPa, at the same time, the system is circulated and fluidized and the temperature is raised to 75-80°C. Add the catalyst, raise the temperature to 85°C and start timing, control the polymerization temperature at ~90°C, stop the reaction after 4 hours, vent and discharge. Weigh and carry out performance test, and the aggregation results are shown in Table 2.

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Abstract

A catalyst for polymerization or copolymerization of ethylene is prepared through dissolving magnesium halide in organic epoxy compound, organic phosphorus compound or inertial diluent, adding alkane educing aid, porous inertial carrier and halide of Ti, and educing. It is possible to add alcohol compound and/or electron donor. Its advantages are high activity and copolymerizing performance, and high sensitivity to hydrogen regulation.

Description

technical field [0001] The present invention relates to a catalyst component for homopolymerization of ethylene or copolymerization of ethylene and other α-olefins, its preparation method, and its application in ethylene polymerization or copolymerization. Background technique [0002] In the late 1970s, Japan’s Mitsui Petrochemical Company and U.S. Monel and other companies successfully developed a titanium-magnesium high-efficiency carrier catalyst with magnesium chloride as a carrier. Due to the use of the carrier, the utilization rate of the active center of the titanium atom was improved, and the polymerization process was simplified. Therefore, the world polyolefin industry has developed rapidly. The preparation method of the catalyst for ethylene polymerization and copolymerization disclosed in JP49-51378 by Japan's Mitsui Petrochemical Company is: in the mineral oil medium, magnesium dichloride and ethanol are reacted to generate MgCl 2 ·6C 2 h 5 OH alcoholate slu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/654C08F10/02
Inventor 陈伟郭子方周俊领郭蕾王洪涛刘月祥王如恩史新波程晓静沈贻芳
Owner CHINA PETROLEUM & CHEM CORP
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