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Synthesis method of zirconocene olefin polymerization catalyst

A technology for olefin polymerization and synthesis methods, which is applied in chemical instruments and methods, metallocenes, organic chemistry, etc. It can solve the problems of complex and harsh conditions, high cost, and high energy consumption, and achieve mild process conditions, low cost, and low energy consumption. Effect

Pending Publication Date: 2022-05-17
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for synthesizing a zirconocene type olefin polymerization catalyst in order to solve the problems of complex and harsh conditions, high cost and high energy consumption in the existing synthesis method of zirconocene type olefin polymerization catalysts
The zirconocene-type olefin polymerization catalyst of the present invention can efficiently solve the problem of controlling the isomerism in the production of metallocene polypropylene, and can catalyze the synthesis of polypropylene with high isomerism

Method used

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  • Synthesis method of zirconocene olefin polymerization catalyst
  • Synthesis method of zirconocene olefin polymerization catalyst
  • Synthesis method of zirconocene olefin polymerization catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Step 1, the synthesis of 2-methyl-3-bromothiophene

[0031]

[0032]Dissolve diisopropylamine (56ml, 363mmol) in 200ml of anhydrous tetrahydrofuran, cool to -78°C, add n-butyllithium (2.5M n-hexane solution, 140ml, 330mmol), after the addition is complete, continue at -78°C Stir for 15min. To the solution containing lithium diisopropylamide (LDA) was added dropwise 3-bromothiophene (50 g, 307 mmol). After the addition was complete, the reactant was transferred to an ice bath, allowed to rise to 0°C naturally, and stirred for another 30 min. The reactant was cooled to -78°C, and iodomethane (21ml, 330mmol) was slowly added dropwise. The reaction mixture was stirred at -78 °C for another 30 min, then warmed to 0 °C and stirred for 1 h. After the reaction was completed, it was quenched with saturated brine, separated, and the aqueous phase was extracted with dichloromethane, washed with water, separated, dried over magnesium sulfate, filtered, and the solvent was rem...

Embodiment 2

[0046] Step 1, the synthesis of 2-methyl-3-bromothiophene

[0047] Dissolve 3-bromothiophene (50g, 307mmol) in 200ml of anhydrous tetrahydrofuran, cool to -78°C, add lithium hexamethyldisilazide (2M tetrahydrofuran solution, 165ml, 330mmol), after the addition is complete, - Stirring was continued for 15 min at 78 °C. Then the reactant was transferred into an ice-water bath, allowed to rise to 0°C naturally, and stirred for another 30 min. The reactant was cooled to -78°C, and iodomethane (21ml, 330mmol) was slowly added dropwise. The reaction mixture was stirred at -78 °C for another 30 min, then warmed to 0 °C and stirred for 1 h. After the reaction was completed, it was quenched with saturated brine, separated, and the aqueous phase was extracted with dichloromethane, washed with water, separated, dried over magnesium sulfate, filtered, and the solvent was removed in vacuo. The residue was distilled under reduced pressure to obtain a colorless oily liquid (38.11 g, 70%)....

Embodiment 3

[0058] Step 1, the synthesis of 2-methyl-3-bromothiophene

[0059] Dissolve 3-bromothiophene (50g, 307mmol) in 200ml of anhydrous tetrahydrofuran, cool to -78°C, add sodium hexamethyldisilazide (2M tetrahydrofuran solution, 165ml, 330mmol), after the addition is complete, - Stirring was continued for 15 min at 78 °C. Then the reactant was transferred into an ice-water bath, allowed to rise to 0°C naturally, and stirred for another 30 min. The reactant was cooled to -78°C, and iodomethane (21ml, 330mmol) was slowly added dropwise. The reaction mixture was stirred at -78 °C for another 30 min, then warmed to 0 °C and stirred for 1 h. After the reaction was completed, it was quenched with saturated brine, separated, and the aqueous phase was extracted with dichloromethane, washed with water, separated, dried over magnesium sulfate, filtered, and the solvent was removed in vacuo. The residue was distilled under reduced pressure to obtain a colorless oily liquid (39.70 g, 73%). ...

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Abstract

The invention relates to a synthesis method of a zirconocene olefin polymerization catalyst, belonging to the technical field of synthesis of organic and high polymer materials. The preparation method comprises the following steps: reacting 3-bromothiophene with strong base, and carrying out methylation reaction with methyl iodide to obtain 2-methyl-3-bromothiophene; the preparation method comprises the following steps: carrying out a Friedel-Crafts acylation reaction, a Nashroff cyclization reaction and a Suzuki coupling reaction on 2, 5-dimethyl-3-phenyl-5, 6-dihydrocyclopentane [1, 2-b] thiophene-4-ketone to obtain 2, 5-dimethyl-3-phenyl-5, 6-dihydrocyclopentane [1, 2-b] thiophene-4-ketone; carrying out reduction and elimination to obtain 2, 5-dimethyl-3-phenyl-6-cyclopentene [1, 2-b] thiophene; and finally, carrying out silylation and zircon salt coordination to obtain the target zirconocene type olefin polymerization catalyst. The synthesis conditions are relatively mild, the synthesis method is low in cost and low in energy consumption, and industrial production of the catalyst is facilitated.

Description

technical field [0001] The invention belongs to the technical field of synthesis of metal organic and polymer materials, and in particular relates to a synthesis method of a zirconocene type olefin polymerization catalyst. Background technique [0002] Polypropylene is the fastest growing polyolefin resin in recent years. The key factor for its rapid development lies in the rapid development of polymerization catalyst related technologies. Catalyst plays a pivotal role in polypropylene production technology. Catalyst system has great influence on the properties of polypropylene products (such as relative molecular weight and distribution, product shape, random polymer content, etc.), conversion rate, production conditions (such as operating temperature) And the amount of catalyst residue in the product has an important impact. [0003] In the research and development of polypropylene catalysts, improving the catalytic activity and stereoselectivity of catalysts and improvin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/00C08F110/06C08F4/642C07F17/00
CPCC08F10/00C08F110/06C07F17/00C08F2500/15C08F4/6428
Inventor 王博徐宇航段亚轩
Owner JILIN UNIV
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