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Vanadium complex based on acenaphthene quinone diimine ligand and preparation method and application of vanadium complex

A technology of acenaphthoquinone bisimine and vanadium complexes, which is applied in the preparation of vanadium complexes and the application field of olefin polymerization catalysts, and can solve the problems of large amounts of catalysts and co-catalysts, high molecular weight of catalytic products, and high degree of polymer branching. problem, to achieve the effect of high molecular weight, high product yield and high catalytic activity

Inactive Publication Date: 2019-03-01
HEBEI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the shortcomings of the α-diimine metal catalysts in the prior art, such as low catalytic activity, low polymer molecular weight, large amount of catalyst and cocatalyst, high degree of polymer branching, etc., the present invention provides a kind of acenaphthoquinone based bis The vanadium complex of imine ligands can be used as a catalyst for olefin polymerization through the effective combination of ligands and metals. It has the advantages of high catalytic activity, high molecular weight of catalytic products, and low degree of branching.

Method used

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  • Vanadium complex based on acenaphthene quinone diimine ligand and preparation method and application of vanadium complex
  • Vanadium complex based on acenaphthene quinone diimine ligand and preparation method and application of vanadium complex
  • Vanadium complex based on acenaphthene quinone diimine ligand and preparation method and application of vanadium complex

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Embodiment 1

[0035] Preparation of vanadium complexes based on acenaphthoquinone bis-imine ligands, the structural formula of which is shown in formula I, R = 2,6-dimethylphenyl. Reaction scheme and concrete process are as follows:

[0036]

[0037] Under nitrogen protection, at room temperature, 20 mL of anhydrous toluene was added to the ligand 1,2-bis[(2,6-dimethylphenyl)imino]-acenaphthene (0.194 g, 0.5 mmol) to dissolve it, Then add VCl slowly 3 (THF) 3 (0.187 g, 0.5 mmol) in 10 mL of toluene, stirred for 12 hours. After the reaction, the liquid was concentrated to 5 mL under reduced pressure, 10 mL of hexane was added, filtered under nitrogen protection, the filter cake was washed twice with 2 mL of hexane, and 0.252 g of solid powder was obtained after vacuum drying with a yield of 82%. The elemental analysis formula is C 32 h 31 Cl 3 N 2 OV (%): C, 62.46; H, 5.22; N, 4.45.

Embodiment 2

[0039] Preparation of vanadium complexes based on acenaphthoquinone bis-imine ligands, the structural formula of which is shown in formula I, R = 2,6-diethylphenyl. Reaction scheme and concrete process are as follows:

[0040]

[0041] Under the protection of nitrogen, at room temperature, 20 mL of anhydrous toluene was added to the ligand 1,2-bis[(2,6-diethylphenyl)imino]-acenaphthene (0.222 g, 0.5 mmol) to dissolve it, Then add VCl slowly 3 (THF) 3 (0.187 g, 0.5 mmol) in 10 mL of toluene, stirred for 12 hours. After the reaction, the liquid was concentrated to 5 mL under reduced pressure, 10 mL of hexane was added, filtered under nitrogen protection, the filter cake was washed twice with 2 mL of hexane, and 0.272 g of solid powder was obtained after vacuum drying with a yield of 81%. The elemental analysis formula is C 36 h 39 Cl 3 N 2 OV (%): C, 64.03; H, 5.68; N, 4.06.

Embodiment 3

[0043] Preparation of vanadium complexes based on acenaphthoquinone bis-imine ligands, the structural formula of which is shown in formula I, R = 2,6-isopropylphenyl. Reaction scheme and concrete process are as follows:

[0044]

[0045] Under the protection of nitrogen, add 20 mL of anhydrous toluene to the ligand 1,2-bis[(2,6-diisopropylphenyl)imino]-acenaphthene (0.250 g, 0.5 mmol) at room temperature to dissolve it, Then add VCl slowly 3 (THF) 3 (0.187 g, 0.5 mmol) in 10 mL of toluene, stirred for 12 hours. Concentrate the liquid to 5 mL under reduced pressure, add 10 mL of hexane, filter under nitrogen protection, wash the filter cake twice with 2 mL of hexane, and obtain 0.316 g of solid powder after vacuum drying, with a yield of 87%. The elemental analysis formula is C 40 h 47 Cl 3 N 2 OV (%): C, 65.77; H, 6.60; N, 3.91.

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Abstract

The invention discloses a vanadium complex based on an acenaphthene quinone diimine ligand and a preparation method and application of the vanadium complex. The structural formula of the vanadium complex is shown as the following formula I (please see the specifications for the formula). The vanadium complex based on the acenaphthene quinone diimine ligand is prepared from the acenaphthene quinonediimine ligand and VCl3 (THF)3 through a one-step reaction at the normal temperature, preparation is easy, separation is not needed in the reaction process, and the product yield is high. The vanadium complex based on the acenaphthene quinone diimine ligand has good copolymerization performance, can serve as a catalyst of an olefin polymerization reaction, and is high in catalytic activity, longin life and small in using amount, an obtained polyolefin product is high in molecular weight, narrow in molecular weight distribution, and low in branching degree, and great application prospects areachieved.

Description

technical field [0001] The present invention relates to a complex, in particular to a vanadium complex based on acenaphthoquinone bis-imine ligand, and also to a preparation method of the vanadium complex based on acenaphthoquinone bis-imine ligand and its use as a catalyst for olefin polymerization Applications. Background technique [0002] Polyolefin materials are currently the most widely used synthetic polymer materials and are used in all aspects of production and life in human society. The development of the polyolefin industry mainly relies on the design and production of olefin polymerization catalysts. Because the structure of the catalyst will determine the morphology and properties of the resulting polymer. Among many olefin polymerization catalysts, transition metal catalysts based on α-diimine ligands are a very important class of catalysts. [0003] Since Brookhart reported in 1995 that α-diimine nickel and palladium catalysts (J. Am. Chem. Soc., 1995, 117,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F110/02C08F4/685C08F210/16C08F210/14C07F9/00
CPCC07F9/005C08F110/02C08F210/16C08F4/685C08F210/14
Inventor 郝志强林进郑学忠岳晓辉刘康阎新龙
Owner HEBEI NORMAL UNIV
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