Non-metallocene bidentate double-vanadium complex as well as preparation method and application thereof

A vanadium complex, non-locene technology, applied in the field of non-locene bidentate double vanadium complexes and preparation, can solve the problems of increasing the molecular weight of the polymer, broadening the molecular weight distribution, asymmetric bimetallic structure, etc. The effect of range, good stability and low catalyst cost

Active Publication Date: 2018-06-22
武汉绿本科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

2. The molecular weight of the resulting polymer will generally increase; and due to the possible structural asymmetry of the bimetal, two different active centers will be generated, resulting in a broadening of the molecular weight distribution

Method used

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  • Non-metallocene bidentate double-vanadium complex as well as preparation method and application thereof
  • Non-metallocene bidentate double-vanadium complex as well as preparation method and application thereof
  • Non-metallocene bidentate double-vanadium complex as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Synthesis of bidentate double vanadium complex V1

[0032]

[0033] Add 1 mmol of ligand (L1) to the Schlenk bottle, and then evacuated nitrogen for three times, and added 20 ml of tetrahydrofuran to dissolve the ligand; at 0 °C, the ligand solution was introduced into 10 ml of tetrahydrofuran suspension dissolved with 2 mmol of KH, and the temperature was raised to The reaction was stirred at room temperature for 5 hours; 2 mmol of VCl was added to another schlenk bottle 3 (THF) 3 and 10 ml of tetrahydrofuran; introduce the potassium salt solution of the ligand into VCl at -78 °C 3 (THF)3 In the solution, the temperature was slowly raised to 40 °C and reacted for 36 h, then filtered, concentrated under reduced pressure, slowly added n-hexane to cover the upper layer of the solution, and allowed to stand to obtain a black solid powder with a yield of 76%. Elemental analysis: Theoretical (%): C, 58.64; H, 5.95; N, 2.85; Tested (%): C, 58.32; H, 5.43; N, 3.06.

Embodiment 2

[0035] Synthesis of bidentate double vanadium complex V2

[0036]

[0037] Add 1mmol ligand L2 in Schlenk bottle, replace with nitrogen three times, add 20ml dichloromethane to dissolve the ligand, add dissolved 1mmol VO (O i Pr) 3 10ml of dichloromethane solution, stirred at room temperature for 12 hours, then added 1mmol of o-methylimino vanadium trichloride in dichloromethane solution, then added dropwise 0.2ml of triethylamine, stirred at room temperature for 12 hours, The solution was concentrated to 20 ml, the upper layer was covered with hexane, and after standing, a black solid powder was obtained with a yield of 58%. Elemental analysis: Theoretical value (%): C, 58.44; H, 6.58; N, 4.99; Test value (%): 58.43; H, 6.68; N, 4.55.

Embodiment 3-11

[0039] Synthesis of Bidentate Bivanadium Complexes V3-V11

[0040]

[0041] L3, V3: R=H; L4, V4: R=2- i Pr; L5, V5: R=2,6- i Pr 2 ; L6, V6: R=2-F; L7, V7: R=3-F; L8, V8: R=4-F; L9, V9: R=2,4-F 2 ;L10,V10: R=3,4,5-F 3 ; L11, V11: R=2,3,4,5,6-F 5

[0042] V3

[0043] room temperature N 2 Under atmosphere, add VCl to the dry Schlenk bottle 3 (THF) 3 (0.26g, 0.7mmol), dissolve in 10ml of tetrahydrofuran, add Schiff base bidentate ligand L3 (0.25g, 0.35mmol) and 10ml of tetrahydrofuran to another Schlenk bottle, stir to dissolve the ligand, then slowly dissolve the ligand The tetrahydrofuran solution was introduced into VCl 3 (THF) 3 tetrahydrofuran solution, and after stirring for 10 min, Et was added dropwise to the mixed solution. 3 N (0.1 ml, 0.73 mmol), Et was added 3 The solution turned black after N. Stir at room temperature for 12 h, remove the solvent in vacuo to obtain a black solid, add 5 ml of tetrahydrofuran to dissolve in the glove box, filter out the...

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Abstract

The invention discloses a non-metallocene bidentate double-vanadium complex as well as a preparation method thereof and an application of the non-metallocene bidentate double-vanadium complex in catalyzing homopolymerization of ethylene and catalyzing copolymerization of ethylene and alpha-olefin, cycloolefin, acyclic diene or a polar monomer. The non-metallocene bidentate double-vanadium complexprovided by the invention has novel design, a simple synthetic method, mild reaction conditions and lower catalyst costs; double metal vanadium has a synergistic effect, the complex has extremely highactivity when being used for catalyzing polymerization of the ethylene, wherein the highest activity is higher than 107g / molV*h, and the catalyst has good stability and can maintain higher activity in a wider temperature range for a longer time; and the complex has extremely high activity when being used for catalyzing copolymerization of the ethylene and other olefins, especially the polar monomer, the insertion rate of a comonomer is high and can be regulated and controlled, and therefore the performance of a polymer can be effectively regulated and controlled.

Description

technical field [0001] The invention relates to a non-locene bidentate double vanadium complex, a preparation method and an application, which belong to the technical field of metal organic chemistry and the technical field of polymer materials. Background technique [0002] Polymer materials are one of the pillar industries of the national economy, of which polyolefin has always been the most important product. Polyolefin is an important polymer material with many advantages such as abundant raw materials, low price, easy processing and molding, etc. In addition, in terms of product performance, it has low relative density, chemical resistance, good water resistance; good mechanical strength, Electrical insulation and other characteristics. It can be used to manufacture films, pipes, plates, various molded products, wires and cables, etc. It has a wide range of uses in agriculture, packaging, electronics, electrical, automobiles, machinery, and daily necessities. [0003...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/00C08F4/68C08F110/02C08F210/02C08F210/16C08F210/18
CPCC07B2200/13C07F9/005C08F4/68043C08F110/02C08F210/02C08F210/16C08F210/18
Inventor 谢光勇肖骁罗德荣熊焰张爱清
Owner 武汉绿本科技有限公司
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