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Binuclear ruthenium catalyst as well as preparation method and application thereof

A catalyst, di-nuclear ruthenium technology, applied in the field of organometallic catalysts for olefin polymerization, can solve the problems of catalyst synthesis and purification difficulties, and achieve the effects of easy operation, mild synthesis conditions, and wide sources

Active Publication Date: 2022-07-22
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, it is relatively difficult to synthesize and purify the catalyst in the method of obtaining a cyclic polymer through ring expansion polymerization of a cyclic catalyst

Method used

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  • Binuclear ruthenium catalyst as well as preparation method and application thereof
  • Binuclear ruthenium catalyst as well as preparation method and application thereof
  • Binuclear ruthenium catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A preparation method of a dual-nuclear ruthenium catalyst, comprising the following steps:

[0041] (1) Preparation of dual-nuclear ruthenium catalyst precursor: under the protection of nitrogen flow, weigh 1,10-dibromodecane (201mg, 0.67mmol) into a 15mL Ace pressure-resistant tube, add 5mL of toluene, and then add 2,4, 6-Trimethylphenylimidazole (250 mg, 1.34 mmol), put the Ace pressure-resistant tube in an oil bath, stir at 110 ° C for 12 h, a light yellow reaction solution precipitates a solid, remove the solvent in vacuo, and dissolve the solid in two. Chloromethane becomes a light yellow liquid, which is dropped into diethyl ether to separate out white powder, which is uniformly sonicated and left to stand, repeatedly washed with dichloromethane and diethyl ether, left to stand in a refrigerator, and the solvent is removed in vacuo to obtain a white powder decane even bis-1-(2, 4,6-Trimethylphenyl)-imidazole bromide 293 mg, yield 65%;

[0042] (2) Preparation of ...

Embodiment 2

[0052] A preparation method of a dual-nuclear ruthenium catalyst, comprising the following steps:

[0053] (1) Preparation of dual-nuclear ruthenium catalyst precursor: under the protection of nitrogen flow, weigh 1,5-dibromopentane (154 mg, 0.67 mmol) into a 15 mL Ace pressure-resistant tube, add 5 mL of toluene, and then add 2, 4, 6-Trimethylphenylimidazole (250 mg, 1.34 mmol), put the Ace pressure-resistant tube in an oil bath, stir at 110 ° C for 12 h, a light yellow reaction solution precipitates a solid, remove the solvent in vacuo, and dissolve the solid in two. Chloromethane becomes a light yellow liquid, which is dropped into diethyl ether to separate out white powder, which is uniformly sonicated and left to stand, repeatedly washed with dichloromethane and diethyl ether, left to stand in a refrigerator, and the solvent is removed in vacuo to obtain a white powder of pentane bis-1-(2, 4,6-Trimethylphenyl)-imidazolium bromide 279 mg (69%);

[0054] (2) Preparation of...

Embodiment 3

[0060] A preparation method of a dual-nuclear ruthenium catalyst, comprising the following steps:

[0061] (1) Preparation of binuclear ruthenium catalyst precursor: under the protection of nitrogen flow, 1,4-bis(bromomethyl)benzene (305 mg, 1.15 mmol) was weighed into a 15 mL Ace pressure-resistant tube, 5 mL of dichloromethane was added, and then 2,4,6-Trimethylphenylimidazole (453mg, 2.43mmol) was added, the Ace pressure-resistant tube was placed in an oil bath, and after stirring at 45°C for 12h, a light yellow reaction solution precipitated a solid, and the solid was dissolved in Methanol became a light yellow liquid, which was dropped into diethyl ether to separate out white powder, which was uniformly sonicated and left to stand, repeatedly washed with methanol and diethyl ether, kept in refrigerator, and the solvent was removed in vacuo to obtain a white powder cyclodimethylene bis-1-(2, 4,6-Trimethylphenyl)-imidazole 640 mg (84%);

[0062] (2) Preparation of binuclea...

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Abstract

The invention discloses a binuclear ruthenium catalyst as well as a preparation method and application thereof, the structural general formula of the binuclear ruthenium catalyst is shown in the specification, and the structural formula of Linker is one of the following formulas. The binuclear ruthenium catalyst is used for catalyzing ring-opening metathesis polymerization of cycloolefin, the binuclear ruthenium catalyst comprises different skeleton structures, the ring-opening metathesis polymerization reaction of cycloolefin monomers can be catalyzed through the electronic effects of different skeletons, the topological structure of a polymer can be effectively controlled, and a new strategy is provided for synthesizing cyclic functionalized polyolefin.

Description

technical field [0001] The invention relates to the field of organic metal catalysts for olefin polymerization, in particular to a dual-nuclear ruthenium catalyst and a preparation method and application thereof. Background technique [0002] Ring-opening metathesis polymerization is a very characteristic polymerization method in the preparation of polymer materials: under the action of a catalyst, the double bond of the cyclic olefin is broken and the polymer is formed in a head-to-tail manner. There are two types of representative catalysts for ring-opening metathesis polymerization: the first type, Schrocktype catalysts with molybdenum metal as the catalytic center, these catalysts have the characteristics of high activity and high selectivity for the polymerization of cyclic olefins, and the price is relatively cheap. , but it is sensitive to water and oxygen, has limited functional group tolerance, and is difficult to store; the second category is Grubbs type catalysts ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C08G61/08
CPCC07F15/0053C08G61/08C08G2261/11C08G2261/3327C08G2261/3325C08G2261/418
Inventor 侯小华任飞扬李珍聂金鑫
Owner HEFEI UNIV OF TECH
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