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Method for preparing solid catalyst for olefin polymerization

A solid catalyst and olefin polymerization technology, applied in the field of solid catalysts in the preparation of olefin polymerization catalysts, can solve the problems of low activity, poor copolymerization performance, unsatisfactory catalyst activity and copolymerization performance, etc.

Active Publication Date: 2012-08-01
利和知信新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The catalysts prepared by the above two methods, due to the use of a solution formed by a single magnesium chloride, the solution is highly uniform, and the magnesium chloride microcrystals with a dense structure are arranged in an orderly manner during the precipitation of magnesium chloride particles, and the degree of disorder is low, resulting in a relatively single microporous structure. , so the activity is low and the copolymerization performance is poor
Therefore, with the development of polypropylene technology, the catalyst prepared by this method cannot meet the growing needs in terms of activity and copolymerization performance.

Method used

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  • Method for preparing solid catalyst for olefin polymerization
  • Method for preparing solid catalyst for olefin polymerization

Examples

Experimental program
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Effect test

Embodiment 1

[0050] Preparation of solid catalyst:

[0051] In a stirred 5-neck flask fully replaced by nitrogen, add 5g magnesium chloride, 1g magnesium ethoxide, 30ml toluene, 25ml isooctyl alcohol, 8ml tributyl phosphate and react at 130°C for 2 hours to form a uniform solution. Add 1.7g of phthalic anhydride to the solution, stir the mixture at 130°C for 1 hour, then add 50ml of toluene to the resulting solution and lower the temperature to -20°C, add 60ml of titanium tetrachloride, then heat up to 80°C, and then Add 5ml of diisobutyl phthalate, continue to heat up to 110°C to react for 1 hour, filter off the liquid phase, wash the solid part with 60ml of toluene for 3 times, then use 80ml of toluene and 20ml of titanium tetrachloride mixture to keep the temperature at 110°C Treated three times in 30 hours, filtered, then washed 5 times with 100ml hexane, filtered off the liquid and dried to obtain 5.5g solid powder which was the solid catalyst component, and the analyzed titanium cont...

Embodiment 2

[0057] Preparation of solid catalyst:

[0058] Add 5g magnesium chloride, 1g ethoxymagnesium chloride, 30ml toluene, 25ml isooctyl alcohol, and 8ml tributyl phosphate to a stirring 5-neck flask fully replaced by nitrogen and react at 130°C for 2 hours to form a uniform solution . Add 1.7g of phthalic anhydride to the solution, stir the mixture at 130°C for 1 hour, then add 50ml of toluene to the resulting solution and lower the temperature to -20°C, add 60ml of titanium tetrachloride, then heat up to 70°C, and then Add 5ml of diisobutyl phthalate to react for 1 hour, filter off the liquid phase, wash the solid part with 60ml of toluene 3 times, then treat it with 80ml of toluene and 20ml of titanium tetrachloride mixture at 110°C for 30 hours at a constant temperature for 3 times, filter , and then washed 5 times with 100ml hexane, filtered off the liquid and dried to obtain 5.3g solid powder which was the solid catalyst component, and the analyzed titanium content was 2.21 (...

Embodiment 3

[0061] Preparation of solid catalyst:

[0062] In a stirred 5-neck flask fully replaced by nitrogen, add 5g magnesium chloride, 1g ethoxymagnesium, 30ml toluene, 2ml ethanol, 20ml isooctyl alcohol, 2ml epichlorohydrin, 5ml tributyl phosphate at 100°C After 2 hours of reaction, a homogeneous solution was formed. Add 1.7g of phthalic anhydride to the solution, stir the mixture at 100°C for 1 hour, then add 50ml of toluene to the resulting solution and lower the temperature to -20°C, add 60ml of titanium tetrachloride, then heat up to 60°C, and then Add 5ml of diisobutyl phthalate to react for 1 hour, filter off the liquid phase, wash the solid part with 60ml of toluene 3 times, then treat it with 80ml of toluene and 20ml of titanium tetrachloride mixture at 110°C for 30 hours at a constant temperature for 3 times, filter , and then washed 5 times with 100ml hexane, filtered off the liquid and dried to obtain 5.2g solid powder which was the solid catalyst component, and the anal...

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Abstract

The invention provides a method for preparing a solid catalyst for olefin polymerization. Components of the solid catalyst comprise: a mixture of magnesium chloride and a magnesium compound with the general formula of MgR<2>R<3>; organic compounds which can dissolve a component a, or a mixture thereof; a titanium compound with the following general molecular formula: Ti(OR<1>)nX4-n; a diester of an aromatic dicarboxylic acid, or an aromatic monoester; an aromatic hydrocarbon or an alkane; and a precipitating aid. The preparation method of the solid catalyst comprises the following steps: mixing the component a, a component b, a component e and a component f to form a solution, allowing the solution to contact with a component c, heating to 30-80DEG C, adding a component d, continuously heating to 90-110DEG C, maintaining for 1-3h, filtering out the resulting liquid phase, washing the resulting solid by the component e at least two times, allowing the resulting solid to contact with a mixed solution of the component c and the component e, filtering, washing the resulting material by the component e three to six times, and drying to form the solid catalyst. The solid catalyst synthesized through the method has the advantages of high polymerization activity and good copolymerization, and is suitable for producing copolymer resins with high ethylene contents.

Description

technical field [0001] The invention relates to a method for preparing a solid catalyst in an olefin polymerization catalyst. Specifically, a solution is prepared from a mixture of two or more magnesium compounds, and then contacted with a titanium compound to crystallize magnesium chloride particles and support the active center of the titanium compound to prepare A method for producing solid catalysts in olefin polymerization catalysts. Background technique [0002] By dissolving magnesium chloride in an organic solvent, contacting titanium tetrachloride to precipitate magnesium chloride particles and supporting titanium active centers, the method of preparing a solid catalyst in an olefin polymerization catalyst has been widely used in the polypropylene industry. [0003] For example, Chinese patent ZL88101916.x discloses a solution that dissolves magnesium chloride and phthalic anhydride in isooctyl alcohol and decane, then contacts the solution with titanium tetrachlori...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/00C08F4/654C08F4/651C08F10/02C08F10/06
Inventor 代金松马庆利高勇许新星赵红霞李甜甜陈红艳刘进凯胡强
Owner 利和知信新材料技术有限公司