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Post-transition metal complex, preparation method thereof and polyethylene preparation method

A late transition metal and complex technology, applied in the field of catalysts, can solve the problem of low catalytic activity of late transition metal complexes

Active Publication Date: 2012-11-14
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the existing late transition metal complexes catalyze ethylene polymerization, the catalytic activity of the late transition metal complexes is still low

Method used

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  • Post-transition metal complex, preparation method thereof and polyethylene preparation method
  • Post-transition metal complex, preparation method thereof and polyethylene preparation method
  • Post-transition metal complex, preparation method thereof and polyethylene preparation method

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preparation example Construction

[0053] The present invention also provides a preparation method of the late transition metal complex, which is specifically prepared according to the following method:

[0054]Reacting bis(substituted aniline)-2,6-pyridinedicarboxamide and phosphorus pentachloride in a first organic solvent for the first time to obtain a ligand with the structure of formula (II);

[0055] performing a second reaction between the ligand and a late transition metal halide in a second organic solvent to obtain a late transition metal complex having the structure of formula (I), the late transition metal being cobalt, iron or nickel;

[0056]

[0057] Among them, R 1 and R 1 Each independently selected from hydrogen or C 1 ~ C 10 alkyl;

[0058] R 3 is hydrogen, halogen or C 1~C 10 alkyl;

[0059] The process of obtaining the ligand with the structure of formula (II) is specifically:

[0060] Under the protection of nitrogen, bis(substituted aniline)-2,6-pyridinedicarboxamide and phosphoru...

Embodiment 1

[0076] Dissolve 8.11g (60mmol) of 2,4,6-trimethylaniline and 8.36ml (60mmol) of triethylamine in 50ml of CH 2 Cl 2 , 6.1 g (30 mmol) of pyridinedicarboxylic acid chloride was dissolved in 20 ml of CH 2 Cl 2 In, pyridine dicarboxylic acid chloride / CH 2 Cl 2 The solution was added dropwise to the substituted aniline / CH 2 Cl 2 After reflux for 4 hours, use 100ml of water and 100ml of 1.5M NaCO 3 The solution was washed, and a separatory funnel was used to obtain the lower CH 2 Cl 2 solution, adding MgSO 4 Dry overnight, filter and suck dry, then recrystallize with toluene, filter and dry to obtain the product (5a). Yield 91%. The product (5a) was analyzed by nuclear magnetic resonance, and the characterization results are as follows: 1 H NMR (400MHz, CDCl 3 , δ, ppm): 9.02 (s, 2H, NH), 8.51 (d, 2H, Pyr-H m ), 8.14 (t, 1H, Pyr-H p ), 6.95 (s, 4H, Ar-H), 2.30 (s, 6H, Ar-C p h 3 ), 2.26 (s, 12H, Ar-C o h 3 ); 13 C NMR (100MHz, CDCl 3 , δ, ppm): 161.6, 148.8, 139....

Embodiment 2

[0082] Dissolve 11.94 g (60 mmol) 4-bromo-2,6-dimethylaniline and 8.36 ml (60 mmol) triethylamine in 50 ml CH 2 Cl 2 , 6.1 g (30 mmol) of pyridinedicarboxylic acid chloride was dissolved in 20 ml of CH 2 Cl 2 In, pyridine dicarboxylic acid chloride / CH 2 Cl 2 The solution was added dropwise to the substituted aniline / CH 2 Cl 2 After reflux for 4 hours, use 100ml water and 100ml 1.5M NaCO 3 The solution was washed, and the lower layer of CH was obtained with a separatory funnel 2 Cl 2 solution, adding MgSO 4Dry overnight, filter and suck dry, then recrystallize with toluene, filter and dry to obtain the product (10a), the yield is 86.4%. The product (10a) was analyzed by nuclear magnetic resonance, and the characterization results are as follows: 1 H NMR (400MHz, CDCl 3 , δ, ppm): 8.98 (s, 2H, NH), 8.55 (d, 2H, Pyr-H m ), 8.19 (t, 1H, Pyr-H o ), 7.33 (s, 4H, Ar-H), 2.30 (s, 12H, -CH 3 ); 13 C NMR (100MHz, CDCl 3 , δ, ppm): 161.5, 148.6, 139.5, 137.4, 131.0, 128.2...

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Abstract

The invention provides a post-transition metal complex having a structure shown in a formula (I). The invention also provides a preparation method of the post-transition metal complex, which comprises the following steps: performing first reaction on di(substituted phenylamine)-2,6-pyridine dicarboxamide and phosphorous pentachloride in a first organic solvent to obtain a ligand having a structure shown in a formula (II); and performing second reaction on the ligand and post-transition metal halide in a second organic solvent to obtain the post-transition metal complex having the structure shown in the formula (I). The invention also provides a polyethylene preparation method which comprises the following specific step: under the effects of a cocatalyst and the post-transition metal complex having the structure shown in the formula (I), performing polymerization reaction on ethylene in an organic solvent to obtain polyethylene. The post-transition metal complex provided by the invention has high catalytic activity in catalytic ethylene polymerization.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a late transition metal complex, a preparation method thereof, and a preparation method of polyethylene. Background technique [0002] The development of polyolefin industry is an important symbol of the development of a country's petrochemical industry. Ziegler-Natta catalysts, metallocene catalysts and late transition metal catalysts are the three main research directions of olefin polymerization catalysts. Due to the low price and environmental friendliness of late transition metals, late transition metal catalysts based on olefin polymerization have made great progress in recent years, and late transition metal catalyst systems have gradually become a research hotspot. [0003] Brookhart et al. invented the α-bisimine NN bidentate system, which selected Ni and Pd as the central metal, which showed good activity for ethylene polymerization, and used this system to realize t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/06C07F15/04C07F15/02C08F10/02C08F110/02C08F4/70
CPCY02P20/52
Inventor 张学全刘恒白晨曦张春雨代全权蔡洪光那丽华毕吉福
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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