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Bridged metallocene compound catalyst, and preparation method and application thereof

A metallocene compound and catalyst technology, applied in metallocene, chemical instruments and methods, organic chemistry, etc., can solve the problems of small steric hindrance of substituent groups, fast chain transfer, insufficient rigidity, etc., and achieves wide application prospects, good Effects of catalytic activity, good mechanical properties and processability

Active Publication Date: 2016-10-05
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the inventors have found through research that due to the small steric hindrance of the substituent group in the above structure, the rotation of the metacene group relative to the metal center is not strictly restricted, the rigidity is not high enough, and the chain transfer is fast during the polymerization process, so a higher molecular weight polymer

Method used

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  • Bridged metallocene compound catalyst, and preparation method and application thereof
  • Bridged metallocene compound catalyst, and preparation method and application thereof
  • Bridged metallocene compound catalyst, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) Synthesis of compound a

[0040] Add 0.25mol 3,5-dichlorobenzonitrile and 100mL dry diethyl ether to a 500mL three-neck flask, then add 3.5g metallic lithium at -20°C and react for 20 hours, then add 0.5mol monomethyltrichlorosilane in an ice-water bath After reacting for 6 hours, add 100 mL of distilled water to wash, remove the organic phase with a pear-shaped separatory funnel, wash the water phase with 50 mL of ether three times, combine the organic phases, and wash with anhydrous MgSO 4 Dry, filter, remove the solvent in vacuo, and then recrystallize from ethanol to obtain 22.73 g of white solid, yield 46%.

[0041] Dissolve the above compound in 100 mL of dry tetrahydrofuran, slowly add 0.48 mol cyclopentadiene sodium dropwise at -30°C for 12 hours, remove the solvent in vacuo, and extract the residual solid with 50 mL of ether three times, then place it in an ice-water bath Slowly add 192mL of 2.5M n-butyllithium hexane solution dropwise, then stir at room t...

Embodiment 2

[0047] (1) Synthesis of compound b

[0048] Add 0.12mol 3,5-dichlorobenzonitrile and 80mL dry diethyl ether to a 500mL three-neck flask, then add 1.7g metallic lithium at -20°C and react for 20 hours, then add 0.25mol monomethyltrichlorosilane in an ice-water bath After reacting for 6 hours, add 80 mL of distilled water to wash, remove the organic phase with a pear-shaped separatory funnel, wash the water phase with 30 mL of ether three times, combine the organic phases, and wash with anhydrous MgSO 4 Dry, filter, remove the solvent in vacuo, and then recrystallize from ethanol to obtain 11.53 g of white solid, yield 46%.

[0049] Dissolve the above compound in 100 mL of dry tetrahydrofuran, slowly add 0.24 mol of indenyllithium dropwise at -30°C for 12 hours, remove the solvent in vacuo, extract the residual solid with 50 mL of ether three times, and then slowly drop it in an ice-water bath Add 81mL of 2.5M n-butyllithium hexane solution, then stir at room temperature for 12...

Embodiment 3

[0055] (1) Synthesis of compound c

[0056] Add 0.06mol 3,5-dichlorobenzonitrile and 60mL dry diethyl ether to a 500mL three-necked flask, then add 0.84g metallic lithium at -20°C and react for 20 hours, then add 0.12mol phenyltrichlorosilane in an ice-water bath After reacting for 6 hours, add 60 mL of distilled water to wash, remove the organic phase with a pear-shaped separatory funnel, wash the water phase with 30 mL of ether three times, combine the organic phases, and wash with anhydrous MgSO 4 Dry, filter, remove the solvent in vacuo, and then recrystallize from ethanol to obtain 12.15 g of white solid, yield 44%.

[0057] Dissolve the above compound in 100 mL of dry tetrahydrofuran, slowly add 0.12 mol of sodium cyclocene at -30°C and react for 12 hours, remove the solvent in vacuo, extract the residual solid with 50 ethyl ether three times, and then slowly add 40mL of 2.5M n-butyllithium hexane solution, then stirred at room temperature for 12 hours, filtered, and va...

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Abstract

The invention provides a bridged metallocene compound catalyst, and a preparation method and an application thereof. The chain transfer reaction in a polymerization process is restricted through the space effect by introducing a bridging group with large steric hindrance and high rigidity. The catalyst is used for catalyzing olefin polymerization, has high reaction activity, allows polymers with high molecular weight distribution and high molecular weight to be obtained, and has wide application prospect.

Description

technical field [0001] The invention relates to a metallocene compound catalyst and its application, in particular to a bridged metallocene compound catalyst and its application. Background technique [0002] Metallocene compound catalysts are a new generation of olefin polymerization catalysts after Ziegler-Natta catalysts. Compared with the Ziegler-Natta catalyst, the polymer chain length and comonomer content produced by each active center of the metallocene catalyst are almost the same; the catalyst structure is controllable, and the polyolefin molecular chain can be tailored; Good sensitivity, so polyolefin products with the same fluidity can be obtained under the condition of extremely low hydrogen concentration. [0003] However, the polymers prepared by metallocene catalysts have narrow molecular weight distribution, high shear rate sensitivity, and thus poor processability. Therefore, the preparation of metallocene polyolefins with broad or bimodal distribution is...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F4/6592C07F17/00C08F110/02
Inventor 李丽张鹏王海黄霞徐人威朱博超杨世元王雄韩晓昱乔彤森李广全张平生李朋朋谢克峰刘小燕
Owner PETROCHINA CO LTD
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