Binuclear vanadium catalyst as well as preparation method and application thereof

A nuclear vanadium catalyst and solvent technology, applied in the field of olefin polymerization organometallic catalyst and olefin coordination polymerization, can solve the problems of poor antistatic compatibility, limited application scope, low hygroscopicity, etc., and achieves easy reaction and rich application. , the effect of simple operation

Active Publication Date: 2020-10-09
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is widely used in various fields of industrial production due to its light weight, low price and low hygroscopi

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0043] Example 1

[0044] (1) Preparation of binuclear vanadium trichloride: under the protection of nitrogen, weigh 2,6-dimethyl isocyanate (3.54g, 20mmol) into a Schlenk bottle, add solvent n-octane (15mL), and slowly add trichloro Vanadium, place the Schlenk bottle in an oil bath, stir at 120°C for 12h, filter through diatomaceous earth to obtain a dark green solution, the filtrate is vacuumed to remove the solvent, washed with n-hexane, DCM, stand at -5°C for 6h, Remove the solvent to obtain dark green binuclear vanadium trichloride (3.76g, 40%);

[0045] (2) Preparation of binuclear vanadium trialkylate: Weigh the product of step (1) (150mg, 0.54mmol) into the reaction flask, add solvent toluene (5mL), let stand at -5°C for 1h, slowly add alkyl Lithium reagent (1.91g, 1.62mmol), stirred at room temperature for 6h, filtered through Celite to obtain a reddish brown solution, and removed the solvent in vacuo to obtain a reddish brown oily trialkylate (202mg, 86%);

[0046] (3) Pr...

Example Embodiment

[0050] Example 2

[0051] (1) Preparation of binuclear vanadium trichloride: under the protection of nitrogen, weigh 2,6-dimethyl isocyanate (3.54g, 20mmol) into a Schlenk bottle, add solvent n-octane (15mL), and slowly add trichloro Vanadium, place the Schlenk bottle in an oil bath, stir at 120°C for 12h, filter through diatomaceous earth to obtain a dark green solution, the filtrate is vacuumed to remove the solvent, washed with n-hexane, DCM, stand at -5°C for 6h, Remove the solvent to obtain dark green binuclear vanadium trichloride (3.76g, 40%);

[0052] (2) Preparation of binuclear vanadium trialkylate: Weigh the product of step (1) (150mg, 0.54mmol) into the reaction flask, add solvent toluene (5mL), let stand at -5°C for 1h, slowly add alkyl Lithium reagent (1.91g, 1.62mmol), stirred at room temperature for 6h, filtered through Celite to obtain a reddish brown solution, and removed the solvent in vacuo to obtain a reddish brown oily trialkylate (202mg, 86%);

[0053] (3) Pr...

Example Embodiment

[0057] Example 3

[0058] (1) Preparation of binuclear vanadium trichloride: under the protection of nitrogen, weigh 2,6-dimethyl isocyanate (3.54g, 20mmol) into a Schlenk bottle, add solvent n-octane (15mL), and slowly add trichloro Vanadium, place the Schlenk bottle in an oil bath, stir at 120°C for 12h, filter through diatomaceous earth to obtain a dark green solution, the filtrate is vacuumed to remove the solvent, washed with n-hexane, DCM, stand at -5°C for 6h, Remove the solvent to obtain dark green binuclear vanadium trichloride (3.76g, 40%);

[0059] (2) Preparation of binuclear vanadium trialkylate: Weigh the product (150mg, 0.54mmol) of step (1) into the reaction flask, add solvent toluene (5mL), let stand at -5°C for 1h, slowly add alkyl Lithium reagent (1.91g, 1.62mmol), stirred at room temperature for 6h, filtered through Celite to obtain a reddish brown solution, and removed the solvent in vacuo to obtain a reddish brown oily trialkylate (202mg, 86%);

[0060] (3) Pr...

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Abstract

The invention discloses a binuclear vanadium catalyst. The structural general formula of the catalyst is described in the descriptions of the invention. In the structural general formula, the structural formula of Linker is one of the following formulas described in the descriptions of the invention; R1, R2, R3, R4, R5, R '1, R' 2, R '3, R' 4 and R '5 are one or more of hydrogen atoms, alkyl groups, fluorine atoms, bromine atoms and chlorine atoms. The binuclear vanadium catalyst comprises electron withdrawing groups which can be used for ring-opening metathesis polymerization reaction of monomers with weak catalytic reaction capacity and other cycloolefin monomers; the number of polar groups can be effectively adjusted, the topological structure of a polymer can be effectively controlled,and a new strategy is provided for synthesizing functionalized polyolefin.

Description

technical field [0001] The invention belongs to the fields of olefin polymerization organometallic catalysts and olefin coordination polymerization, and in particular relates to a binuclear vanadium catalyst and a preparation method and application thereof. Background technique [0002] Polyolefin is the polymer material with the largest output in the industry, accounting for more than half of the world's thermoplastic production rate. It is widely used in various fields of industrial production due to its light weight, low price and low hygroscopicity. The poor compatibility of polar polymers or inorganic fillers limits the expansion of its application range. Therefore, the functionalization of non-polar polyolefins, that is, the introduction of polar functional groups or polymer segments in their molecular chains, can significantly improve the flexibility, adhesion, protective properties, and surface properties of polymer materials. Performance, solvent resistance, misci...

Claims

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Application Information

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IPC IPC(8): C08G61/08
CPCC08G61/08C08G2261/11C08G2261/13C08G2261/418C08G2261/3324C08G2261/3321
Inventor 侯小华陈小建高翔聂金鑫周昕玥邹辉周丽
Owner HEFEI UNIV OF TECH
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