2,6-diisopropyl aniline salicylaldiminato nickel, and preparation and application thereof

A technology of diisopropylaniline and propylaniline water, which is applied to 2,6-diisopropylaniline salicylic aldimine nickel and its preparation and application fields, can solve the problems of high cost, difficult to obtain raw materials and the like

Inactive Publication Date: 2012-09-26
PETROCHINA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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  • 2,6-diisopropyl aniline salicylaldiminato nickel, and preparation and application thereof
  • 2,6-diisopropyl aniline salicylaldiminato nickel, and preparation and application thereof
  • 2,6-diisopropyl aniline salicylaldiminato nickel, and preparation and application thereof

Examples

Experimental program
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Embodiment 1

[0016] [O-(3-CH 3 )C 6 h 3 CH=N-2,6-C 6 h 3 i PR 2 ]Ni(PPh 3 )(Ph)(cat1) Preparation

[0017] Under the protection of an inert gas, 3-methyl salicylaldehyde (2.72g, 0.02mol) was dissolved in 100mL ethanol solvent, 2,6-diisopropylaniline (3.8mL, 0.02mol) was added, and in 0.5mL acetic acid Under the action, react at 0°C for 12 hours, and naturally cool to room temperature to obtain light yellow needle-like solid, namely 3-methyl-salicylaldimine ligand. Dissolve 1.6mmol of this ligand in 80mL of tetrahydrofuran, add NaH (38mg, 1.6mmol), react at -20°C for 6 hours, and transfer the supernatant to the metal nickel compound trans-[NiCl(Ph)(PPh 3 ) 2 ] (1.1g, 1.6mmol) in toluene solvent, react at -20°C for 48 hours. After the reaction, the solvent was drained, and the residue was recrystallized with an organic solvent composed of toluene and n-hexane (volume ratio: 1:1) to obtain 10.68 g of a solid catalyst cat with a yield of 62%.

Embodiment 2

[0019] [O-(3-iC 3 h 7 )C 6 h 3 CH=N-2,6-C 6 h 3 i PR 2 ]Ni(PPh 3 )(Ph)(cat2) Preparation

[0020] Under the protection of an inert gas, 3-isopropyl salicylaldehyde (3.28g, 0.02mol) was dissolved in 50mL ethanol solvent, 2,6-diisopropylaniline (4.3mL, 0.023mol) was added, and in 0.5mL Under the action of acetic acid, reacted at 20°C for 10 hours, and naturally cooled to room temperature to obtain light yellow needle-like solid, namely 3-isopropyl-salicylaldimine ligand. Dissolve 2.4mmol of this ligand in 80mL of tetrahydrofuran, add NaH (76mg, 3.2mmol), react at -10°C for 4 hours, and transfer the supernatant to the metal nickel compound trans-[NiCl(Ph)(PPh 3 ) 2 ] (1.1g, 1.6mmol) in toluene solvent, react at -10°C for 36 hours. After the reaction, the solvent was drained, and the residue was recrystallized with an organic solvent composed of toluene and n-hexane (volume ratio: 2:1) to obtain 20.60 g of a solid catalyst cat with a yield of 52%.

Embodiment 3

[0022] [O-(3-CH 3 )-(5-Br)C 6 h 3 CH=N-2,6-C 6 h 3 i PR 2 ]Ni(PPh 3 )(Ph)(cat3) Preparation

[0023] Under the protection of an inert gas, 3-methyl-5-bromosalicylaldehyde (4.28g, 0.02mol) was dissolved in 50mL ethanol solvent, 2,6-diisopropylaniline (4.5mL, 0.024mol) was added, Under the action of 0.5 mL of acetic acid, reacted at 40°C for 8 hours, and naturally cooled to room temperature to obtain a light yellow needle-like solid, namely 3-methyl-5-bromosalicylaldimine ligand. Dissolve 3.2 mmol of this ligand in 80 mL of tetrahydrofuran, add NaH (115 mg, 4.8 mmol), react at -5°C for 3 hours, and transfer the supernatant to the metal nickel compound trans-[NiCl(Ph)(PPh 3 ) 2 ] (1.1g, 1.6mmol) in toluene solvent, react at 0°C for 24 hours. After the reaction, the solvent was drained, and the residue was recrystallized with an organic solvent composed of toluene and n-hexane (volume ratio: 4:1) to obtain 30.86 g of solid catalyst cat with a yield of 70%.

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Abstract

The invention relates to a 2,6-diisopropyl aniline salicylaldiminato nickel, and preparation and application thereof. The preparation method comprises the steps of: adding 2,6-diisopropyl aniline into salicylaldehyde with substituent by a molar ratio of 1:1-1.5; reacting under effect of acetate for 60-80 DEG C; dissolving the obtained salicylaldiminato in a solvent and adding NaH by a molar ratio of 1:1-6; reacting at -20-5 DEG C; transferring a clear liquid to an aromatic hydrocarbon or ether solvent of trans-[NiCl(Ph)(PPh3)2] by a molar ratio of 1-3:1; reacting at -20-40 DEG C; pumping out the solvent; and recrystallizing by an organic solvent to obtain the catalyst. The catalyst is used for catalysis of ethene polymerization and adjusts molecular weight, molecular weight distribution and polymer branched structure of an ethene polymer through adjusting polymerization conditions or hydroxy ortho-position substituent of salicylaldiminato.

Description

technical field [0001] The invention relates to a kind of 2,6-diisopropylaniline salicylaldimine nickel, its preparation and the single-component method of using the complex for ethylene polymerization. Background technique [0002] At present, olefin polymerization catalysts based on early transition metals, such as Ziegler-Natta catalysts and metallocene catalysts, have many advantages, but they all need to be initiated by co-catalysts to carry out olefin polymerization, and these catalysts are prone to be water, oxygen and polar groups. inactivated. With the in-depth research on a new generation of non-metallocene and late-transition metal olefin polymerization catalysts, a class of single-component, high-efficiency olefin polymerization catalysts without cocatalysts has gradually attracted people's attention. In 1998, the Grubbs research group of the California Institute of Technology reported a kind of neutral nickel complex, which can catalyze the polymerization of et...

Claims

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Application Information

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IPC IPC(8): C07F15/04C08F10/02C08F4/80
Inventor 陈谦张丹枫王斯晗王筱玲李建忠刘国敏于部伟孙悦黄付玲邓筱娟王秀绘王力搏张志翔张文超刑士轩马逢伯于相国邴淑秋王桂芝何玉莲李华隋婷韩雪梅王亚丽张德顺
Owner PETROCHINA CO LTD
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