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Olefinic polymerization catalyst carried by carrier of sphere MgCl-alcohol-organic complexing agent and preparation method

A technology of organic complexing agent and polyolefin catalyst, which is applied in the field of catalyst preparation, can solve the problems affecting the shape of catalyst particles, and achieve the effects of moderate looseness, easy control of particle size and simple preparation process

Inactive Publication Date: 2005-01-12
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

TiCl 4 The stirring method loaded on the carrier will affect the particle shape of the catalyst. The commonly used methods are mechanical stirring method and magnetic stirring method, but the mechanical stirring will break the catalyst particles and affect the particle shape of the catalyst.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) carrier preparation

[0025] The carrier was prepared according to the method described in Example 1 of Patent Application No.: 02136543.1.

[0026] (2) Preparation of catalyst

[0027] Take 2.7g of the above-mentioned spherical carrier and slowly add it into a reaction bottle filled with 66ml of titanium tetrachloride and pre-cooled to -30°C, react at low temperature for 20 minutes, and the final temperature does not exceed 0°C. Gradually raise the temperature to 60°C, add 0.6ml of diisobutyl phthalate (DIBP), continue to heat up to 130°C, react for 2 hours, remove the upper liquid after cooling down, and then add 46ml of TiCl 4 , gradually raised the temperature to 130°C, and reacted for another 2 hours, then removed the upper liquid, and washed several times with n-hexane at 80°C until the washing liquid was clear. The resulting solid was vacuum dried to obtain a spherical catalyst with a Ti content of 8.96%.

[0028] (3) Propylene polymerization

[0029] Car...

Embodiment 2

[0031] (1) Carrier preparation is the same as in Example 1.

[0032] (2) Preparation of catalyst

[0033] Take 2.3 g of the spherical carrier and slowly add it into a reaction flask filled with 56 ml of titanium tetrachloride and precooled to -20° C., and react at low temperature for 30 minutes. Gradually raise the temperature to 60°C, add 0.5ml of di-n-octyl phthalate (DNOP), continue to heat up to 130°C, react for 1.5 hours, remove the upper liquid after cooling down, and then add 40ml of TiCl 4 , gradually raised the temperature to 130°C, and reacted for another 2 hours, then removed the upper liquid, and washed several times with n-hexane at 80°C until the washing liquid was clear. The resulting solid was vacuum dried to obtain a spherical catalyst with a Ti content of 3.04%.

[0034] (3) Propylene polymerization

[0035] Slurry polymerization under atmospheric pressure, petroleum ether as solvent, AlEt 3 / TiCl 4 The molar ratio is 120, the DPDMS / Ti molar ratio is 2.4...

Embodiment 3

[0037] (1) The carrier preparation steps are the same as in Example 1.

[0038] (2) Preparation of catalyst

[0039] Take 2.0 g of the spherical carrier and slowly add it into a reaction flask filled with 56 ml of titanium tetrachloride and precooled to -30° C., and react at low temperature for 15 minutes. Gradually raise the temperature to 60°C, add 0.46ml of diethyl phthalate (DEP), continue to heat up to 120°C, react for 2 hours, remove the upper liquid after cooling down, and then add 30ml of TiCl 4 , gradually raised the temperature to 120°C, and reacted for another hour, then removed the upper liquid, and washed several times with n-hexane at 80°C until the washing solution was clear. The resulting solid was vacuum dried to obtain a spherical catalyst with a Ti content of 2.93%.

[0040] (3) Copolymerization of propylene and dodecene

[0041] Slurry polymerization under atmospheric pressure, petroleum ether as solvent, AlEt3 / TiCl 4 The molar ratio is 120, the DPDMS / T...

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PUM

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Abstract

The invention discloses an defin polymerization catalyst loaded on spherical MgCl2-alcohol-organic complexing agent camier and its preparation method. Said method includes the following steps: under the protection of argon gas using TiCl4 and MgCl2-alcohol-organic complexing agent spherical carrier, stirring them at -30 deg.c-0 deg.C in reaction still and making them produce reaction for 10-30 min., heating to 60 deg.C-80 deg.C, adding internal doner residues, and more heating to 90 deg.C-140 deg.C, thermostatically stirring and making reaction for 1-3 hr., then removing liquid phase, adding TiCl4 to make treatment once, and removing liquod phase, washing by using solvent, removing solvent, vacuum drying so as to obtain spherical catalyst. Said spherical catalyst uses spherical MgCl2-alcohol-organic complexing agent as carrier, and the preparation process of said catalyst is retatively simple, and small in environmental pollution. Said invention can effectively regulate grain size of catalyst and its distribution by controlling grain size of spherical MgCl2-alcohol-organic copmlexing agent carrier and its distribution, after the olefin is catalyzed and polymerized, the spherical polyolefin can be obained.

Description

Technical field [0001] The present invention relates to the preparation method of catalyst, relate in particular to a kind of spherical MgCl 2 -Alcohol-organic complexing agent carrier supported olefin polymerization catalyst and preparation method. Background technique [0002] Polyolefins, especially polypropylene and its copolymers, have a wide range of applications due to their low cost, light weight and good processing properties. The demand is constantly increasing, and the global production capacity is also increasing. The rapid development and continuous improvement of polyolefin production has benefited from the continuous advancement of catalysts. By designing and preparing spherical catalysts, spherical homopolymers and copolymers can be obtained, and the obtained polymer particles can be directly applied to processing and production without granulation process. [0003] Currently commonly used preparation of MgCl 2 The method of spherical carrier has spray-dry...

Claims

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Application Information

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IPC IPC(8): C08F4/02C08F4/76C08F10/00
Inventor 叶朝阳王立马振利王剑峰
Owner ZHEJIANG UNIV
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