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Dicaryon pyrene (alpha-diimine) nickel olefin catalyst and preparation method and application thereof

An olefin catalyst, catalyst technology, applied in chemical instruments and methods, nickel organic compounds, organic chemistry, etc., can solve the problems of low molecular weight and low branching degree of polyethylene, and achieve high molecular weight, high polymerization activity and high branching degree. Effect

Active Publication Date: 2018-11-23
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The catalyst has high activity in catalyzing ethylene polymerization, but the molecular weight and branching degree of the prepared polyethylene are low, and the characteristics of (α-diimine) nickel catalyst for preparing highly branched polyethylene through "chain walking" are not sufficient. play out

Method used

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  • Dicaryon pyrene (alpha-diimine) nickel olefin catalyst and preparation method and application thereof
  • Dicaryon pyrene (alpha-diimine) nickel olefin catalyst and preparation method and application thereof
  • Dicaryon pyrene (alpha-diimine) nickel olefin catalyst and preparation method and application thereof

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Experimental program
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preparation example Construction

[0029] The preparation method of dinuclear pyrene (alpha-diimine) nickel olefin catalyst comprises the steps:

[0030] (1) Tetraketone compound C1 and 2 equivalents of 2,6-diisopropylaniline undergo ketoamine condensation reaction to obtain compound C2:

[0031]

[0032] (2) Compound C2 and 2 equivalents of 2,6-dimethylaniline undergo ketoamine condensation reaction to obtain ligand C3:

[0033]

[0034] (3) Compound C2 and 2 equivalents of 2,6-diethylaniline undergo ketoamine condensation reaction to obtain ligand C4:

[0035]

[0036] (4) Compound C2 performs ketoamine condensation reaction with 1 equivalent of 2,6-diethylaniline, and then performs ketoamine condensation reaction with 1 equivalent of 2,6-dimethylaniline to obtain ligand C5:

[0037]

[0038] (5) Under anhydrous and oxygen-free conditions, ligands C3, C4, and C5 are mixed with 2 equivalents of (DME)NiBr 2 The complexation will obtain catalysts 1, 2, and 3 in the following formula respectively. ...

Embodiment 1

[0055] Synthesis of Ligand C3

[0056] Under nitrogen atmosphere and 85°C, compound C2 (0.58g, 1mmol) was added to a three-necked flask containing 50mL of acetonitrile, stirred mechanically, and after reflux at 85°C for half an hour, 10mL of acetic acid was added, and the reflux was continued for two and a half hours . 0.25 g (2 mmol) of 2,6-dimethylaniline were added. Stop the reaction after 24 hours, stand still, and cool naturally. The precipitate was washed with 5×50 mL of n-heptane, and then dried under vacuum at 70° C. for 48 hours. 0.652 g of the product was obtained with a yield of 83%.

[0057] 1 H-NMR (400MHz, CDCl 3 ,δin ppm): 8.16(d,4H,Py-H),7.72(d,2H,Py-H),7.43-7.51(d,4H,Ar-H),7.04-7.12(d,8H,Ar- H),2.87(sept,4H,CH(CH 3 ) 2 ),2.34(s,12H,CH 3 ),0.86~1.20(dd,24H,CH(CH 3 ) 2 ).

[0058] Elem.Anal.Calcd.For C 56 h 58 N 4 : C, 85.50%; H, 7.38%; N, 7.12%. Found: C, 85.56%; H, 7.32%; N, 7.19%.

[0059] ESI-MS: m / z 787.50 ([M+H] + )

Embodiment 2

[0061] Synthesis of Ligand C4

[0062] Under nitrogen atmosphere and 85°C, compound C2 (0.58g, 1mmol) was added to a three-necked flask containing 50mL of acetonitrile, stirred mechanically, and after reflux at 85°C for half an hour, 10mL of acetic acid was added, and the reflux was continued for two and a half hours . 0.3 g (2 mmol) 2,6-diethylaniline was added. Stop the reaction after 24 hours, stand still, and cool naturally. The precipitate was washed with 5×50 mL of n-heptane, and then dried under vacuum at 70° C. for 48 hours. 0.682 g of the product was obtained with a yield of 81%.

[0063] 1 H-NMR (400MHz, CDCl 3 ,δin ppm): 8.16(d,4H,Py-H),7.72(d,2H,Py-H),7.51-7.57(d,4H,Ar-H),7.11-7.12(d,8H,Ar- H),2.87(sept,4H,CH(CH 3 ) 2 ),2.60(q,8H,CH 2 ),1.25(T,12H,CH 3 ),0.86~1.20(dd,24H,CH(CH 3 ) 2 ).

[0064] Elem.Anal.Calcd.For C 56 h 58 N 4 : C, 85.51%; H, 7.84%; N, 6.65%. Found: C, 85.58%; H, 7.89%; N, 6.61%.

[0065] ESI-MS: m / z 843.0 ([M+H] + )

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Abstract

The invention relates to the field of olefin catalytic polymerization, and aims to provide a dicaryon pyrene (alpha-diimine) nickel olefin catalyst and a preparation method and application thereof. The chemical structural formula of the catalyst is as shown in the formula I. 2,6-diisopropyl aniline is introduced beside the nickel metal center innovatively so as to inhibit a polymerization growth chain to generate a chain transfer reaction to a monomer. The dicaryon pyrene (alpha-diimine) nickel olefin catalyst provided by the invention can prepare polyethylene with the higher molecular weightand the higher branching degree, and meanwhile the polymerization activity is higher. The formula I is shown in the description.

Description

technical field [0001] The invention relates to the field of catalytic polymerization of olefins, in particular to a binuclear pyrene (α-diimine) nickel olefin catalyst and a preparation method and application thereof. Background technique [0002] Polyolefin is a basic material related to the national economy and people's livelihood, and because of its excellent performance, various varieties, easy availability and low price of raw materials, it is widely used in various fields such as industry, agriculture and national defense. The development and application of new catalysts is one of the core driving forces to promote the progress and development of the polyolefin industry, and is the key to controlling the structure and performance of polyolefins. [0003] The (α-diimine) nickel olefin catalyst can catalyze the polymerization of ethylene to obtain branched polyethylene. Researchers have done a lot of research and improvement on this type of catalyst in order to obtain ...

Claims

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Application Information

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IPC IPC(8): C08F10/00C08F10/02C08F110/02C08F4/70C07F15/04
CPCC07F15/045C08F10/00C08F10/02C08F110/02C08F2410/03C08F4/7006C08F2500/01Y02P20/52
Inventor 傅智盛张昊范志强
Owner ZHEJIANG UNIV
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