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Ziegler-Natta polyethylene catalyst with wide molecular weight distribution, and preparation method thereof

A wide molecular weight distribution, Ziegler technology, applied in the field of catalysts, can solve the problems of low catalytic activity, complicated preparation process, high preparation cost, etc., and achieve the effect of stable polymerization reaction and easy reaction process

Inactive Publication Date: 2010-11-10
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The bimetallic catalyst and co-catalyst are used in ethylene polymerization reaction, and the polyethylene produced has a wide molecular weight distribution between 7 and 20, but the catalytic activity of this catalyst is low, only 400 to 1000g PE / g cat, due to the use of more complex organic precursors, the preparation process is complicated and the preparation cost is high

Method used

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  • Ziegler-Natta polyethylene catalyst with wide molecular weight distribution, and preparation method thereof
  • Ziegler-Natta polyethylene catalyst with wide molecular weight distribution, and preparation method thereof
  • Ziegler-Natta polyethylene catalyst with wide molecular weight distribution, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] A. Preparation of main catalyst

[0062] (1) Treatment of silica carrier

[0063] The temperature of silicon dioxide (Grace Davison 955) was continuously raised to 600° C. under nitrogen fluidization, and kept for 10 hours, and then gradually cooled to room temperature before use. Add thermally activated silica (SiO 2 ) 20g, add 40ml hexane and 1.3ml triethylaluminum (Et 3 A1) Stir to form a slurry, mix and react for 2.5 hours, and then dry to obtain a silica carrier with good fluidity.

[0064] (2) Preparation of new ecological magnesium chloride

[0065] In a 500ml five-necked reaction flask equipped with a stirrer, condenser, dropping funnel and heating device, add 300ml of n-hexane and 7.2500g of magnesium powder, and 64ml of chlorobutane (BuCl ) was added dropwise in the reaction flask, after the dropwise addition was completed, the reaction was continued at 60° C. for 4.5 hours to obtain a black new ecological magnesium chloride solid suspension. The solvent ...

Embodiment 2

[0078] (1) Treatment of silica carrier

[0079] Method and consumption ratio are with embodiment 1 (1).

[0080] (2) Preparation of new ecological magnesium chloride

[0081] In a 500ml five-necked reaction flask equipped with a stirrer, condenser, dropping funnel and heating device, add 250ml of n-hexane and 6.4g of magnesium powder, and add 56ml of chlorobutane dropwise at 65°C for 3.5 hours Into the reaction bottle, after the dropwise addition, the reaction was continued at 63° C. for 5 hours to obtain a black new ecological magnesium chloride solid suspension. The solvent was distilled off at 70° C., and after cooling, 300 ml of tetrahydrofuran was added to the reaction flask, and stirred evenly to obtain a black solution. Sampling and analysis yielded Mg=0.863 mol / l, Cl=1.58 mol / l, and Cl / Mg=1.83.

[0082] The structural formula that obtains new ecological magnesium chloride is: (MgBuCl) 0.20 (MgCl 2 )

[0083] (3) Preparation of the main catalyst component

[0084...

Embodiment 3

[0094] (1) Treatment of silica carrier

[0095] Method and consumption are with embodiment 1 (1).

[0096] (2) Preparation of new ecological magnesium chloride

[0097] In a 500ml five-necked reaction flask equipped with a stirrer, condenser, dropping funnel and heating device, add 300ml of n-hexane and 10.5g of magnesium powder, and add 68ml of chlorobutane dropwise at 60°C for 3.5 hours into the reaction bottle, after the dropwise addition, the reaction was continued at 45° C. for 4.5 hours to obtain a black new ecological magnesium chloride solid suspension. The solvent was distilled off at 70° C., and after cooling, 240 ml of tetrahydrofuran was added to the reaction flask and stirred evenly to obtain a black solution. Sampling and analysis obtained: Mg=1.75 mol / l, Cl: 2.66 mol / l, Cl / Mg=1.52. The structural formula that obtains new ecological magnesium chloride is: (BuMgCl) 0.92 (MgCl 2 )

[0098] (3) Preparation of the main catalyst component

[0099] In the five-n...

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Abstract

The invention relates to a Ziegler-Natta polyethylene catalyst used for vinyl polymerization, a preparation method and an application thereof. The main catalyst component of vinyl polymerization catalyst is prepared by the reaction with the following method: using magnesium powder as raw material for reaction to generate new ecological halide; leading the new ecological halide to have complexation reaction with titanium compound and treated silicon dioxide under the condition that electron donor exists; leading complexation product to have contact reaction with alkyl aluminium compound in alkane solvent system; and after heating and drying, having complexation reaction on the product of the contact reaction and polymer containing polar functional group in the alkane solvent system. The polyethylene catalyst is formed by the main catalyst component and cocatalyst metal organic compound, is higher in polymerization activity, and has the advantage that the produced polymer has wider molecular weight distribution.

Description

technical field [0001] The invention relates to a catalyst for ethylene polymerization, a preparation method and an application in ethylene polymerization. Background technique [0002] A traditional Ziegler-Natta catalyst contains a main catalyst and a co-catalyst. The main catalyst is usually a transition metal element compound of Group IVB of the periodic table, and the most commonly used is a Ti compound. Cocatalysts are usually organoaluminum compounds, commonly used are Al(C 2 h 5 ) 3 , Al(C 2 h 5 ) 2 Cl, Al 2 (C 2 h 5 ) 3 Cl 3 Wait. [0003] The performance of Ziegler-Natta catalysts used in the synthesis of polyethylene has been greatly improved after several generations of development. For example, the birth of supported catalysts improves the polymerization activity of Ziegler-Natta catalysts. Activated magnesium chloride is the most effective carrier for Ziegler-Natta catalysts. In the prior art, active magnesium chloride and inert carriers with high ...

Claims

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Application Information

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IPC IPC(8): C08F4/649C08F10/02
CPCY02P20/52
Inventor 吴文清肖明威阳永荣叶晓峰王靖岱蒋斌波郭宇李阳阳
Owner CHINA PETROLEUM & CHEM CORP
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