Beta-diketone monoimine vanadium catalyst containing trifluoromethyl radical for olefinic polymerization and its preparation method and uses

A technology of diketone monoimine vanadium olefin and polymerization catalyst, which is applied in the field of β-diketone monoimine vanadium olefin polymerization catalyst and its preparation, and can solve problems such as weak ability and poor high temperature resistance

Inactive Publication Date: 2008-07-30
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recently, the Japanese scientist Nomura et al. reported a vanadium catalyst with high catalytic activity (Macromolecules 2005, 38: 5905-5913), but its ability to catalyze olefin copolymerization is not strong, and its high temperature resistance is poor.

Method used

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  • Beta-diketone monoimine vanadium catalyst containing trifluoromethyl radical for olefinic polymerization and its preparation method and uses
  • Beta-diketone monoimine vanadium catalyst containing trifluoromethyl radical for olefinic polymerization and its preparation method and uses
  • Beta-diketone monoimine vanadium catalyst containing trifluoromethyl radical for olefinic polymerization and its preparation method and uses

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 1,1,1-trifluoro-5,5-dimethyl-2,4-hexanedione 7.85g, equivalent to 40mmol, aniline 3.73g, equivalent to 40mmol, methanol 15mL, Formic acid 1mL, heated to reflux for 24h. The solvent methanol was distilled off with a rotary evaporator, and petroleum ether containing 1% ethyl acetate was used as eluent, and the residue was subjected to column chromatography to obtain 5.64 g of white solid Schiff's base, with a yield of 52%. According to mass spectrometry, the molecular ion peak m / e is 271. Elemental analysis found values: C, 61.78%; H, 5.90%; N, 5.19%; theoretical value (C14H16F3NO): C, 61.98%; H, 5.94%; N, 5.16%.

[0035] Under nitrogen protection, 0.54 g of the Schiffer base obtained in Example 1, equivalent to 2 mmol, and 20 mL of anhydrous tetrahydrofuran were added to a dry 100 mL reaction flask, stirred at room temperature for 10 min, and cooled to -78°C. Within 5 minutes, 1.375 mL of a 1.60 mol / L n-butyllithium hexane solution, equivalent to 2.2 mmol, was adde...

Embodiment 2

[0037] 4.29 g of o-methylaniline, equivalent to 40 mmol, was used to replace the aniline in Example 1, and the experimental operation was the same as in Example 1 to obtain 5.48 g of white solid Schiff's base, with a yield of 48%. According to mass spectrometry, the molecular ion peak m / e is 285. Elemental analysis found values: C, 63.32%; H, 6.31%; N, 4.94%; theoretical value (C15H18F3NO): C, 63.15%; H, 6.36%; N, 4.91%.

[0038] Using 0.57 g of Schiffer's base prepared in Example 2, which is equivalent to 2 mmol to replace the Schiffer's base obtained in Example 1, the experimental operation is the same as in Example 1, and brown β-diketone monoimine vanadium olefin containing trifluoromethyl is obtained The polymerization catalyst was 0.54 g, and the yield was 49%. According to mass spectrometry, the molecular ion peak m / e is 550. Elemental analysis found values: C, 50.10%; H, 5.99%; N, 2.53%; theoretical value (C22H33Cl2F3N03V): C, 50.19%; H, 6.04%; N, 2.55%.

Embodiment 3

[0040] 5.41 g of 2,4,6-trimethylaniline, equivalent to 40 mmol, was used to replace the aniline in Example 1, and the experimental operation was the same as in Example 1 to obtain 5.26 g of white solid Schiff's base, with a yield of 42%. According to mass spectrometry, the molecular ion peak m / e is 313. The measured value of elemental analysis; C, 65.29%; H, 7.12%; N, 7.42%; theoretical value (C17H22F3NO): C, 65.16%; H, 7.08%; N, 4.47%.

[0041] Using 0.63 g of Schiffer's base prepared in Example 3, which is equivalent to 2 mmol to replace the Schiffer's base obtained in Example 1, the experimental operation is the same as in Example 1, to obtain brown β-diketone monoimine vanadium olefin containing trifluoromethyl The polymerization catalyst was 0.52 g, and the yield was 45%. According to mass spectrometry, the molecular ion peak m / e is 578. Elemental analysis found values: C, 51.72%; H, 6.48%; N, 2.39%; theoretical value (C25H37Cl2F3NO3V): C, 51.91%; H, 6.45%; N, 2.42%.

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Abstract

The invention discloses a beta- diketone imines vanadium olefin polymerized catalyst containing trifluoromethyl and the it's preparing method and its application. The beta- diketone compound containing trifluoromethyl carries out condensation reaction with aniline or its derivative in methanol solution under catalytic action of aminic acid, and gets schiff base; carrying out reaction with said schiff base and butyl lithium on waterless and anaerobic condition to get anion ligand; proceeding coordination reaction with said anion ligand and vanadium trichloride on waterless and anaerobic condition to get final product. The catalyst can catalyze ethane polymerization, combined polymerization of ethane with norbornene, combined polymerization of ethane with alpha- ethane or norbornene, under action of diethyl aluminium chloride or modified methyl aluminoxanes.

Description

technical field [0001] The invention relates to a β-diketone monoimine vanadium olefin polymerization catalyst containing trifluoromethyl and a preparation method. [0002] The present invention also relates to the application of the β-diketone monoimine vanadium olefin polymerization catalyst containing trifluoromethyl group in catalyzing ethylene polymerization, ethylene and norbornene copolymerization, ethylene and α-olefin copolymerization. Background technique [0003] In the 1950s, Ziegler and Natta independently discovered that the catalytic system composed of early transition metals and alkylaluminum compounds can effectively catalyze the homopolymerization and copolymerization of olefins. Since then, polyolefin catalysts have brought revolution to people’s lives. Sexual changes. As one of the most important polymer materials, polyolefin has been widely used in industry, agriculture, national defense, transportation and people's daily life. Catalysts are composed o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/02C08F4/685
Inventor 李悦生段轶群李彦国张贵宝唐丽明张所波
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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