Catalyst component preparation method and catalyst for vinyl polymerization

A technology for ethylene polymerization and catalyst, which is applied to the preparation of catalyst components for ethylene polymerization and the field of catalysts, can solve the problems of irregular catalyst particles, impact on production environment, low polymer melt index, etc., and achieve good ethylene polymerization catalysis The effect of activity, good hydrogen regulation performance and simple preparation method

Active Publication Date: 2013-02-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation process of most of these catalysts is relatively cumbersome, and usually includes the step of reacting the organoaluminum compound with the spray-dried catalyst precursor
[0004] Chinese patent CN1140722 discloses a catalyst prepared by first dissolving magnesium chloride solid, and then reacting with titanium halide to co-precipitate and precipitate. The catalyst is used in the gas phase polymerization process. The catalyst particles are irregular and the sphericity is relatively poor.
[0005] European patent EP0601524 discloses a catalyst prepared by preforming magnesium chloride to support active components. During the preparation of the catalyst, it needs to be treated with a large amount of titanium tetrachloride at a high temperature of 120°C to 140°C, which is easy to damage the equipment. Severe corrosion occurs, which has a serious impact on the production environment; the catalyst is used in the gas-phase polymerization process, and it is easily broken when the polymerization reaction activity is high, resulting in a large amount of polymer fine powder, which usually requires an increase in the pre-polymerization process; in addition, the catalyst’s Poor sensitivity to hydrogen adjustment, that is, under similar polymerization conditions, the hydrogen partial pressure is similar, but the melt index of the obtained polymer is significantly lower

Method used

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  • Catalyst component preparation method and catalyst for vinyl polymerization

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Effect test

Embodiment 1

[0036] Preparation method of spherical catalyst component

[0037] Under nitrogen protection, add 3.85 g of spherical magnesium chloride alcoholate into a 250 ml glass reactor, add 40 ml of n-hexane, stir to form a slurry, cool down to -60°C with a low-temperature bath, and slowly add 24 ml within one hour 2 mol / L triethylaluminum hexane solution, maintained at -60°C for 4 hours. The liquid was then pressure filtered and the solid was washed twice with 40 ml of hexane. Then the solid was stirred with 30 ml of hexane to form a slurry, and at 0°C, 20.0 ml of a hexane solution of titanium tetrachloride (containing 0.5 ml of titanium tetrachloride) was slowly added dropwise, stirred and reacted for 1 hour, and then slowly heated to 50 The reaction was maintained with stirring at °C for 2 hours. After the reaction was finished, it was allowed to stand, and the liquid was filtered out, washed twice with 40 milliliters of hexane, and the solid was blown dry with nitrogen to obtain ...

Embodiment 2

[0041] The preparation method of spherical catalyst component is as follows:

[0042] Under nitrogen protection, add 3.94 g of spherical magnesium chloride alcoholate into a 250 ml glass reactor, add 40 ml of n-hexane, stir to form a slurry, cool down to -60°C with a low-temperature bath, and slowly add 14 ml within one hour 2 mol / L triethylaluminum hexane solution, maintained at -60°C for 4 hours. Then the temperature was slowly raised to 0° C., and 20.0 ml of titanium tetrachloride hexane solution (containing 0.5 ml of titanium tetrachloride) was slowly added dropwise, and the reaction was stirred for 1 hour, and then the temperature was slowly raised to 50° C. and kept stirring for 2 hours. After the reaction was finished, it was allowed to stand, and the liquid was filtered out, washed twice with 40 milliliters of hexane, and the solid was blown dry with nitrogen to obtain 3.67 grams of a solid catalyst component with good fluidity, and its average particle size was 53.4 m...

Embodiment 3

[0046] The preparation method of spherical catalyst component is as follows:

[0047] Under nitrogen protection, add 3.78 g of spherical magnesium chloride alcoholate into a 250 ml glass reactor, add 40 ml of n-hexane, stir to form a slurry, cool down to -10°C with a low-temperature bath, and slowly add 24 ml within one hour 2 mol / L triethylaluminum hexane solution, maintained at -10°C for 4 hours. The liquid was then pressure filtered and the solid was washed twice with 40 ml of hexane. Then the solid was stirred with 30 ml of hexane to form a slurry, and at 0°C, 20.0 ml of a hexane solution of titanium tetrachloride (containing 0.5 ml of titanium tetrachloride) was slowly added dropwise, stirred and reacted for 1 hour, and then slowly heated to 50 The reaction was maintained with stirring at °C for 2 hours. After the reaction was finished, let it stand, filter the liquid, wash twice with 40 milliliters of hexane, and dry the solid with nitrogen to obtain 3.45 grams of soli...

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Abstract

The invention relates to a catalyst component preparation method and a catalyst for vinyl polymerization. The method comprises the following step of: after proper chemical modification is performed on a magnesiumhalide alcoholic compound at a certain temperature, directly loading active ingredients such as titanium tetrachloride and the like to prepare the catalyst which can be applied to vinyl slurry polymerization and gas-phase polymerization. The method is simple and is easy to control. When catalyzing vinyl polymerization, the catalyst prepared by the method has high hydrogen regulation sensitivity; catalyst particles are compact, are difficult to crush, have good shapes, are spherical and have relatively high catalytic activity; and the obtained polymer particles are spherical and have a small amount of fine powder.

Description

technical field [0001] The invention relates to a preparation method of a catalyst component for ethylene polymerization and a catalyst thereof. Background technique [0002] In the development of olefin polymerization catalysts, Ziegler-Natta catalysts with good particle shape have always been one of the goals pursued by people, especially in the gas phase polyethylene process, which is particularly important because of the good particle shape Ziegler-Natta catalysts form polymers in fine particle form so that they do not clog equipment. [0003] US Patent No. 4,293,673 discloses a catalyst prepared by using a composite carrier of silica gel and magnesium chloride. The catalyst has high activity when used in a gas phase polymerization process, and the prepared ethylene polymer has a good particle shape. However, the preparation process of most of these catalysts is relatively cumbersome, and usually includes the step of reacting an organoaluminum compound with a spray-drie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/658C08F4/645C08F10/02
Inventor 王世波高克京刘东兵吕新平邢宝泉王丽莎毛炳权
Owner CHINA PETROLEUM & CHEM CORP
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