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Benzylamine side arm-containing half-metallocene chromium (IV) complex and application thereof

A single metallocene, benzylamine group-containing technology, applied in the application of catalyzing ethylene homopolymerization and ethylene/α-olefin copolymerization, in the field of benzylamine sidearm single metallocene chromium complexes, which can solve problems such as synthesis difficulties , to achieve the effect of high catalytic activity, moderate copolymerization performance and stable structure

Inactive Publication Date: 2017-12-01
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

(References a: Y. Liang, Glenn P.A. Yap, Arnold L. Rheingold, and Klaus H. Theopold. Organometallics, 1996, 15, 5284-5286. b: A. Dohring, J. Gohre, P. W. Jolly. Organometallics, 2000, 19:388-402.c: Emrich R, Heinemann O, Jolly P W, etal.Organometallics,1997,16(8):1511-1513; A.Hohring,V.R.Jensen,P.W.Jolly.W.Thiel,J.C.Weber.Macromol .Symp.,2001,173:117-121; A.Hohring,V.R.Jensen,P.W.Jolly.Organometallics,2001,20:2234-2245.d,e:Enders M,FernándezP,Ludwig G,et al.Organometallics,2001 ,20(24):5005-5007.f:Zhang L,Gao W,Tao X,et al.Organometallics,2010,30(3):433-440.) Because there is no suitable chromium (IV) raw material, the synthesis is difficult , a chromium(IV) olefin polymerization catalyst similar to a sidearm mono-titanocene(IV) catalyst has not been reported

Method used

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  • Benzylamine side arm-containing half-metallocene chromium (IV) complex and application thereof
  • Benzylamine side arm-containing half-metallocene chromium (IV) complex and application thereof
  • Benzylamine side arm-containing half-metallocene chromium (IV) complex and application thereof

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Experimental program
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Effect test

Embodiment 1

[0022] The preparation of embodiment 1 complex 1

[0023]Under nitrogen protection, 2-(isopropyl-nitrogen-methyl)phenyl-tetramethylcyclopentadiene (ligand 1) (0.700g, 2.60mmol) in tetrahydrofuran (20mL ) solution was added dropwise a n-hexane solution of n-butyllithium (2.16mL, 5.20mmol). After the addition was complete, the resulting reaction mixture was stirred at this temperature for an additional hour, then the mixture was allowed to rise to room temperature and continued stirring at this temperature for three hours, which was slowly added to 2 equivalents of CrCl 3 (THF) 3 in tetrahydrofuran solution, stirred overnight, removed the solvent, added 20 mL of toluene to the ampoule, filtered to remove insoluble matter, and removed the toluene in the filtrate in vacuo. Then 20 mL of hexane was added to the ampoule for ultrasonic solidification and filtered. The obtained solid was washed with cold hexane (5 mL×2), and then recrystallized with THF / hexane. 0.541 g of the pure ...

Embodiment 2

[0025] The preparation of embodiment 2 complex 2

[0026] Under nitrogen protection, at -78°C, 2-(cyclohexyl-nitrogen-methyl)phenyl-tetramethylcyclopentadiene (ligand 2) (0.805g, 2.60mmol) in tetrahydrofuran (20mL) A solution of n-butyllithium (2.16 mL, 5.20 mmol) in n-hexane was added dropwise to the solution. After the addition was complete, the resulting reaction mixture was stirred at this temperature for an additional hour, after which the mixture was allowed to warm to room temperature and stirred at this temperature for an additional three hours. Add it to 2 equivalents of CrCl 3 (THF) 3 The tetrahydrofuran solution was stirred overnight, the solvent was removed, 20 mL of toluene was added to the ampoule, the insoluble matter was removed by filtration, and the toluene in the filtrate was removed in vacuo. Then 20 mL of hexane was added to the ampoule for ultrasonic solidification and filtered. The obtained solid was washed with cold hexane (5 mL×2), and then recrysta...

Embodiment 3

[0027] The preparation of embodiment 3 complex 3

[0028] Under nitrogen protection, at -78°C, 2-(phenyl-nitrogen-methyl)phenyl-tetramethylcyclopentadiene (ligand 3) (0.789g, 2.60mmol) in tetrahydrofuran (20mL) A solution of n-butyllithium (2.16 mL, 5.20 mmol) in n-hexane was added dropwise to the solution. After the addition was complete, the resulting reaction mixture was stirred at this temperature for an additional hour, after which the mixture was allowed to warm to room temperature and stirred at this temperature for an additional three hours. Add it to 2 equivalents of CrCl 3 (THF) 3 The tetrahydrofuran solution was stirred overnight, the solvent was removed, 20 mL of toluene was added to the ampoule, the insoluble matter was removed by filtration, and the toluene in the filtrate was removed in vacuo. Then 20 mL of hexane was added to the ampoule for ultrasonic solidification and filtered. The obtained solid was washed with cold hexane (5 mL×2), and then recrystalliz...

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Abstract

The invention discloses a benzylamine side arm-containing half-metallocene chromium (IV) complex and application thereof, belonging to the technical field of olefin polymerization catalysts. The benzylamine side arm-containing half-metallocene (IV) complex has a following structure expression: the structure expression is shown in the description. The benzylamine side arm-containing half-metallocene (IV) complex can be applied to catalysis of ethylene homopolymerization or catalysis of the copolymerization of ethylene and alpha-olefin by taking the benzylamine side arm-containing half-metallocene (IV) complex as a main catalyst and taking alkylaluminoxane or a mixture of aluminum alkyl and an organoboron adjuvant as a catalyst promoter. The half-metallocene chromium (IV) complex provided by the invention has the advantages that the structure is stable, the heat resistance is good, the service life is long, the catalytic activity is high, the copolymer molecular weight is high and the like.

Description

technical field [0001] The invention belongs to the technical field of olefin polymerization catalysts, in particular to a monometallocene chromium (IV) complex containing benzylamino group side arm and its application in catalyzing ethylene homopolymerization and ethylene / α-olefin copolymerization. Background technique [0002] Compared with traditional Ziegler-Natta catalysts, metallocene olefin polymerization catalysts have excellent performance in many aspects. The catalyst structure can be designed according to the needs, and then the composition, structure, stereoregularity, molecular weight and molecular weight of polyolefin products can be controlled. Distribution and other performance indicators. Constrained geometry complexes containing sidearm mono-titanocene(IV) and mono-chromocene(III) complexes have been found to be suitable for catalyzing the copolymerization of ethylene and α-olefins to produce linear low-density polyethylene. In the past two decades, A vari...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F11/00C08F110/02C08F210/16C08F210/14C08F4/69
CPCC07F11/00C08F110/02C08F210/16C08F4/69C08F210/14
Inventor 母瀛宋婷婷李丰史喆
Owner JILIN UNIV
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