Preparation method and application for heterogeneous olefin polymerization catalyst

A technology for olefin polymerization and catalyst, applied in the field of olefin polymerization catalyst and its preparation, can solve problems such as no reports, and achieve the effects of easy separation and purification, high activity, and high catalytic activity

Inactive Publication Date: 2013-02-27
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there is no report to the compoun...

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  • Preparation method and application for heterogeneous olefin polymerization catalyst
  • Preparation method and application for heterogeneous olefin polymerization catalyst

Examples

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Embodiment 1

[0024] A method for preparing a heterogeneous olefin polymerization catalyst, using a magnesium-containing compound as a carrier, and using a sulfonylamine compound as an internal electron donor, the preparation steps are as follows:

[0025] 1) Preparation of sulfonylamine compounds:

[0026] Add 10mmol 3,4-dimethoxyaniline and 20mmol triethylamine into a 100ml schlenk bottle, add 40ml dichloromethane under a nitrogen atmosphere, stir and dissolve thoroughly, then place it in a DFY-80 low temperature reaction bath to -78 ℃, dropwise add 10ml of dichloromethane solution with a concentration of 2mmol / ml trifluoromethanesulfonic anhydride, the reaction mixture is fully stirred during the dropwise addition, rise to room temperature after the dropwise addition, and stir at room temperature or heated to solvent reflux for 2h to The reaction is sufficient, the reaction mixture is washed twice with distilled water, each time with one volume of distilled water, after the above two was...

Embodiment 2

[0035] A preparation method of a heterogeneous olefin polymerization catalyst, the preparation steps are as follows:

[0036] 1) Preparation of sulfonylamine compounds: the same as in Example 1;

[0037] 2) Preparation of heterogeneous olefin polymerization catalyst:

[0038] Pre-cool 60ml of titanium tetrachloride to -15°C, then add 2g of magnesium alkoxide MgCl 2 (EtOH) 2.5 Add the pre-cooled titanium tetrachloride to carry out the first titanium loading reaction, then raise the temperature to 0°C at a heating rate of 1°C / 5min, and then heat it to 40°C after naturally rising to room temperature, and add 0.099g of the above-mentioned sulfur Acyl amine compounds, at the same time, 0.067g dibutyl phthalate (a commonly used internal electron donor) was added to investigate the effect of compound use. After half an hour of reaction, it was raised to reflux temperature, stirred and heated for 2 hours, and the reaction solution was brownish black, the upper layer liquid is brown...

Embodiment 3

[0042] A preparation method of a heterogeneous olefin polymerization catalyst, the steps are as follows:

[0043] 1) Preparation of sulfonylamine compounds:

[0044] Add 10mmol 2,4-dimethoxyaniline and 20mmol triethylamine to a 100ml schlenk bottle, add 40ml dichloromethane under a nitrogen atmosphere, stir and dissolve thoroughly, and place it in a DFY--80 low-temperature reaction bath to -78 ℃, dropwise add 10ml of dichloromethane solution with a concentration of 2mmol / ml trifluoromethanesulfonic anhydride, the reaction mixture is fully stirred during the dropwise addition, rise to room temperature after the dropwise addition, and stir at room temperature or heated to solvent reflux for 2h to The reaction is sufficient, the reaction mixture is washed twice with distilled water, each time with one volume of distilled water, after the above two washings and liquid separation, the organic phase is collected, fully dried with anhydrous magnesium sulfate, and the solvent is evapo...

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Abstract

The invention relates to a preparation method for a heterogeneous olefin polymerization catalyst. The preparation method comprises the following steps: 1) mixing substituting arylamine with triethylamine, adding dichloromethane as a solvent, placing into a low-temperature reaction bath and cooling, and then dropwise adding a dichloromethane solution of trifluoromethanesulfonic anhydride and fully stirring, and after heating up, stirring under a backflow condition till fully reacting, and then washing, separating solution, drying, distilling and washing hexane, thereby obtaining a sulfonyl amine compound, and 2) adding a magnesium-containing compound into pre-cooled titanium tetrachloride, performing titanium loading reaction for the first time, heating up, and then adding the sulfonyl amine compound and reacting for a half hour, filtering out the supernatant, adding the titanium tetrachloride and performing the titanium loading reaction for the second time, filtering out the supernatant, washing and drying, thereby obtaining the heterogeneous olefin polymerization catalyst. The preparation method provided by the invention has the advantages that the preparation and reaction of the sulfonyl amine compound as an inner fed electron body are simple; the products are easily separated and purified; the catalyst has higher catalytic activity for olefin polymerization reaction; and the catalyzed alpha-olefin polymerization product has higher stereoregularity.

Description

technical field [0001] The invention relates to an olefin polymerization catalyst and its preparation, in particular to a preparation method and application of a heterogeneous olefin polymerization catalyst. Background technique [0002] The Z-N catalyst system currently used in industry is mainly MgCl 2 ·ID·TiCl 4 / AlEt 3 / ED, the catalyst system is widely used in the polyolefin synthesis process due to its high efficiency and high stereospecificity. Among them, the internal electron donor ID is added in the catalyst preparation process, and the development of internal electron donor compounds promotes the continuous renewal of catalysts. [0003] The internal electron donors of Z-N polypropylene catalysts discovered earlier are monoester compounds, that is, the internal electron donors of the third-generation catalysts, mainly p-methylbenzoate ethyl ester (PMEB), ethyl benzoate (EB), etc. Aromatic monoester compounds. The catalyst with monocarboxylic acid ester as the...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F4/649C07C311/09C07C303/38
Inventor 崔春明王亮张建颖王航
Owner NANKAI UNIV
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