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Vinyl polymerization catalyst and preparing method thereof

A technology of ethylene polymerization and catalyst, which is applied in the field of ethylene polymerization catalyst and its preparation, which can solve the problems of affecting the shape of final polymer particles, poor reaction stability, and high initial polymerization activity, and achieve increased strength, concentrated particle size distribution, and stable polymerization reaction. Effect

Active Publication Date: 2015-09-30
SHANGHAI RES INST OF CHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, hollow particles will inevitably appear in this technology, which will affect the particle morphology of the final polymer
Moreover, due to the high initial activity of the polymerization, the reaction stability is poor, and it is difficult to control

Method used

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  • Vinyl polymerization catalyst and preparing method thereof
  • Vinyl polymerization catalyst and preparing method thereof
  • Vinyl polymerization catalyst and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Catalyst preparation:

[0053] (1) At room temperature and under the protection of nitrogen, add 80ml of hexane solution of 0.8186mol / L dibutylmagnesium compound, 80ml of hexane and 2.428g of triethylaluminum to a 0.5 liter reactor with electromagnetic stirring , and stirred for 0.5 hours. Then, a solution consisting of 19.468 g of diethylhexanol and 40 ml of hexane was slowly added with a metering pump at a constant speed for 35 minutes, and the reaction was maintained for 1 hour after the addition. Finally, 6.1 g of epichlorohydrin was added, the temperature was raised to 50° C., and the reaction was kept for 2 hours to obtain magnesium complex solution A;

[0054] (2) Cool the reactor to -25°C, slowly add the solution formed by 11.42g of titanium tetrachloride and 40ml of hexane with a metering pump at a constant speed, the addition time is 45 minutes, and keep it at this temperature for 2 hours after the addition is completed. Obtain solution B;

[0055] (3) Afte...

Embodiment 2

[0063] Catalyst preparation:

[0064] (1) At room temperature and under the protection of nitrogen, add 70ml of heptane solution of butyloctylmagnesium compound with a concentration of 1.0336mol / L to a 0.5 liter reactor with electromagnetic stirring, 80ml of n-heptane and triisobutyl Aluminum 8.14g, stirred and reacted for 0.5 hours. Then, a solution consisting of 26.66 g of diethylhexanol and 40 ml of heptane was slowly added with a metering pump at a constant speed for 1.0 hr, and the reaction was maintained for 2 hours after the addition was completed. Finally, 6.8g of tetrahydrofuran was added, the temperature was raised to 50°C, and the reaction was kept for 2 hours to obtain magnesium complex solution A;

[0065] (2) Cool the reaction kettle to -15°C, slowly add the solution formed by 7.16g of titanium tetrachloride and 30ml of heptane with a metering pump at a constant speed, the addition time is 0.5 hours, and keep it at this temperature for 3 hours after the addition...

Embodiment 3

[0072] Catalyst preparation:

[0073] (1) At room temperature and under the protection of nitrogen, add 80ml of hexane solution of dibutylmagnesium compound with a concentration of 0.8186mol / L, 80ml of hexane and 3.86 g, stirring the reaction for 1 hour. Then, a solution consisting of 9.77 g of isobutanol and 40 ml of hexane was slowly added with a metering pump at a constant speed for 35 minutes, and the reaction was maintained for 1 hour after the addition was completed. Finally, 13.4g of epichlorohydrin was added, the temperature was raised to 50°C, and the reaction was kept for 2 hours to obtain magnesium complex solution A;

[0074] (2) Cool the reactor to -30°C, slowly add the solution formed by 23.1g of titanium tetrachloride and 60ml of hexane with a metering pump at a constant speed, the addition time is 1.5 hours, keep the reaction at this temperature for 2 hours after the addition is complete, Obtain solution B;

[0075] (3) After replacing the nitrogen in the re...

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Abstract

The invention relates to vinyl polymerization catalyst and a preparing method thereof. A dialkyl magnesium compound, an aluminum alkyl compound, an alcohol compound and an organic epoxy compound reach with one another through the catalyst to obtain a magnesium compound solution, then titanium compound reacts with the magnesium compound solution, the obtained solution reacts with alph-olefin, solid particles containing prepolymer are obtained, the solid particles react with linear-chain halogenated alkane, and the final catalyst is obtained. Compared with the prior art, the catalyst is high in polymerization activity, stable in reaction, sensitive in hydrogen regulation and high in stacking density, the obtained polymer grains are narrowly distributed, and the number of fine powder is small.

Description

technical field [0001] The invention relates to a catalyst and a preparation method thereof, in particular to an ethylene polymerization catalyst and a preparation method thereof. Background technique [0002] Ziegler-Natta catalysts are widely used in the polymerization of ethylenically unsaturated monomers. It is composed of IV-VI transition metal compounds on the periodic table as main catalysts and I-III metal compounds as co-catalysts. [0003] Ziegler-Natta catalysts that are widely used in industry can be divided into two types. One uses an inorganic inert carrier to support active magnesium chloride and titanium compounds. For example, silicon dioxide is one of the most used inert carriers. This type of catalyst has high mechanical strength, stable and easy-to-control reaction, and the obtained polymer particles have good morphology. For example, in invention patents CN1223267 and CN1268520, silica is used as a carrier, magnesium, titanium compounds and other activ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/02C08F4/649C08F4/658C08F4/651
Inventor 余世炯肖明威叶晓峰
Owner SHANGHAI RES INST OF CHEM IND
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