Preparation method of catalyst for ethylene polymerization

A catalyst and polyethylene technology, applied in the field of polyethylene catalyst preparation, can solve the problems of low solubility, unsatisfactory catalyst polymerization efficiency, high content, etc., achieve stable reaction, easy temperature control, and increase the effect of loading capacity

Active Publication Date: 2014-01-22
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solubility of inorganic magnesium compounds in this type of catalyst is low in the electron donor component, which leads to a high content of inorganic components such as silica gel in the catalyst solid component, which limits the loading capacity of the active component of the catalyst to a certain extent. , leading to catalyst polymerization efficiency is still not satisfactory

Method used

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  • Preparation method of catalyst for ethylene polymerization

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Experimental program
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Effect test

Embodiment 1

[0020] 1. Catalyst preparation

[0021] Add 50ml of dichloromethane, 8.1g of C 2 h 5 OCl and 10.1g triethylamine and 9.5g anhydrous magnesium chloride, react at -10°C for 1 hour, add 20g triethylaluminum to the system, react at 50°C for 2 hours, then add 300ml tetrahydrofuran, react for 2 hours , filter out a small amount of solid components at the bottom, and leave the supernatant for later use.

[0022] Add 2g of smoky silica gel to the above solution, keep stirring at 40°C for 1 hour, then introduce it into the spray dryer under the protection of nitrogen, set the inlet temperature of the spray dryer to 140°C, and the outlet temperature of the slurry material to 40°C, adjust the atomization airflow and the power of the slurry feed pump, so that the outlet temperature of the spray dryer is stabilized at about 90°C for spraying to obtain a microspherical catalyst carrier powder with an average particle size of 25 μm.

[0023] Take 5g of the above-mentioned microspherical c...

Embodiment 2

[0027] 1. Catalyst preparation

[0028] Add 50ml of dichloromethane, 10.8g of C 6 h 5 OCl and 10.7g triethylamine and 9.5g anhydrous magnesium chloride, react at room temperature for 1 hour, add 20g triethylaluminum, react at 60°C for 2 hours, then add 380ml ethyl acetate, react for 2 hours, filter A small amount of solid components at the bottom were discarded, and the supernatant was reserved for future use.

[0029] Add 2g of smoky silica gel to the above solution, keep stirring at 40°C for 1 hour, then introduce it into the spray dryer under the protection of nitrogen, set the inlet temperature of the spray dryer to 140°C, and the outlet temperature of the slurry material to 40°C, adjust the atomization airflow and the power of the slurry feed pump, so that the outlet temperature of the spray dryer is stabilized at about 90°C for spraying to obtain a microspherical catalyst carrier powder with an average particle size of 25 μm.

[0030] Take 5g of the above-mentioned mi...

Embodiment 3

[0034] 1. Catalyst preparation

[0035] Add 50ml of dichloromethane, 10.8g of C 6 h 5 OCl and 18.5g tributylamine and 9.5g anhydrous magnesium chloride, react at room temperature for 1 hour, add 30g diethylaluminum chloride, react at 45°C for 2 hours, then add 400ml ethyl benzoate, react for 2 hours Finally, filter out a small amount of solid components at the bottom, and leave the supernatant for future use.

[0036] Add 4g of smoky silica gel to the above solution, keep stirring at 40°C for 1 hour, then introduce it into the spray dryer under the protection of nitrogen, set the inlet temperature of the spray dryer to 140°C, and the outlet temperature of the slurry liquid to 40°C, adjust the atomization The air flow and the power of the slurry feed pump make the spray dryer outlet temperature stable at about 90°C for spraying. The microspherical catalyst carrier powder with an average particle diameter of 25 μm was obtained.

[0037]Take 5g of the above-mentioned microsph...

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Abstract

The invention discloses a preparation method of a catalyst for ethylene polymerization. By adopting a spray preparation process, the method comprises the following steps: firstly, carrying out pretreatment on anhydrous magnesium halide and compounds with general formulae of ROX and NR<1>3, wherein R and R<1> in the general formulae are C1-10 alkyl, X is halogen, the reaction temperature is -50 DEG C to 50 DEG C, the reaction time is 0.5-10 hours, and the molar ratio of anhydrous magnesium halide to ROX to NR<1>3 is 1:(1-5):(1-5); preparing a mother liquor from pretreated carrier magnesium halide and a titanium compound, and an electron donor; mixing with proper inorganic filler, and contacting active components of the titanium compound to obtain the catalyst after spray forming. The crystal morphology of the carrier magnesium halide can be obviously improved by a pretreatment process of the carrier and the compounds with the general formulae; the loading amount of the active component of the catalyst is improved; the catalyst is especially suitable for ethylene polymerization, and is stable to react in a polymerization process, easy in temperature control, free of a sticky kettle phenomenon, and easy for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a polyethylene catalyst. Background technique [0002] Since the development of high-efficiency polyethylene catalysts in the 1970s, polyethylene catalyst preparation technology has made great progress, and a variety of catalyst preparation systems have been formed. The early grinding method, suspension impregnation method, etc. were gradually replaced by chemical reaction methods in recent years due to the problems of carrier morphology and handling, and the effective loading of catalyst active components on the carrier was low. Catalyst carriers have also gradually transitioned from direct use in the early stage to chemical treatment to improve the shape and performance of the carrier and improve the indicators of polymer products. [0003] The method of preparing supported catalysts has also gradually transitioned from high-speed stirring method, high-gravity method, capillary extrusion method, etc. ...

Claims

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Application Information

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IPC IPC(8): C08F10/02C08F4/658C08F4/649C08F4/646
Inventor 黄安平朱博超贾军纪李振昊李振宇李艳芹高琳谢克锋宋赛楠张平生刘文霞陈雪蓉郝萍
Owner PETROCHINA CO LTD
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