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Symmetrical seven-membered imino pyridine complex containing large steric hindrance substituent groups for preparing polyethylene wax, and preparation method and application of symmetrical seven-membered imino pyridine complex

A complex and alkyl technology, applied in the field of symmetrical seven-membered ring pyridineimine complexes, can solve the problem that polyethylene cannot be used as polyethylene wax, etc.

Active Publication Date: 2019-11-05
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the polyethylene catalyzed by existing catalysts cannot be used as polyethylene wax, especially food-grade polyethylene wax
Furthermore, it is difficult for existing catalysts to meet the requirements of maintaining high catalytic activity at high temperatures, such as 100°C

Method used

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  • Symmetrical seven-membered imino pyridine complex containing large steric hindrance substituent groups for preparing polyethylene wax, and preparation method and application of symmetrical seven-membered imino pyridine complex
  • Symmetrical seven-membered imino pyridine complex containing large steric hindrance substituent groups for preparing polyethylene wax, and preparation method and application of symmetrical seven-membered imino pyridine complex
  • Symmetrical seven-membered imino pyridine complex containing large steric hindrance substituent groups for preparing polyethylene wax, and preparation method and application of symmetrical seven-membered imino pyridine complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] Example 1. Preparation of α,α'-bis(2,4-dimethyl-6-benzhydrylbenzimine)-2,3:5,6-bis(pentamethylene)pyridine dichloride Ferrous[Fe1](R 1 is methyl, R 2 is methyl, R 3 for benzhydryl)

[0081]

[0082] 0.234g (1.0mmol) α,α'-dioxo-2,3:5,6-bis(pentamethylene)pyridine compound represented by formula (II-1), 1.15g (4.0mmol) 2,4 -Dimethyl-6-benzhydrylaniline and 0.199g (1.0mmol) FeCl 2 4H 2 O was dissolved in 10 mL of acetic acid, under nitrogen atmosphere, heated and stirred to reflux for 6 h, the reaction solution was concentrated, a large amount of ether was added, precipitated, and the precipitate was collected by filtration, then the precipitated substrate was dissolved in methanol, the solution was concentrated to the minimum volume, and again A large amount of diethyl ether was added and a precipitate was collected by filtration and washed with a large amount of diethyl ether. After drying, a light green powder (0.695 g, 76.5%) was obtained, which was Fe1 comple...

Embodiment 2

[0086] Example 2. Preparation of α,α'-bis(2-methyl-4,6-bis(benzhydryl)phenylimine)-2,3:5,6-bis(pentamethylene)pyridine bis Cobaltous chloride [Fe2] (R 1 is methyl, R 2 , R 3 for benzhydryl)

[0087]

[0088] Basically the same as the method in Example 1, the difference is that: under the condition of keeping the same molar number of reactants, the aniline participating in the reaction is 2-methyl-4,6-bis(benzhydryl)aniline, and light green is obtained after drying Powder (0.485g, 40%) is Fe2 complex.

[0089] The structural confirmation data are as follows:

[0090] FT-IR (KBr, cm -1 ): 2868(w), 1597(ν C=N )(s), 1555(w), 1494(s), 1447(s), 1338(m), 1256(s), 1207(m), 1151(m), 1077(m), 1030(m), 998(w), 969(m), 828(w), 778(w), 743(w), 698(s).

[0091] Elemental Analysis: C 81 h 71 Cl 2 FeN 3 (1213.23) Theoretical value: C, 80.19; H, 5.90; N, 3.46%. Experimental value: C, 80.00; H, 5.85; N, 3.35%.

Embodiment 3

[0092] Example 3. Preparation of α,α'-bis(2-ethyl-4,6-bis(benzhydryl)phenylimine)-2,3:5,6-bis(pentamethylene)pyridine bis Cobaltous chloride [Fe3] (R 1 is ethyl, R 2 , R 3 for benzhydryl)

[0093]

[0094] Basically the same as the method in Example 1, the difference is that: under the condition of keeping the same molar number of reactants, the aniline participating in the reaction is 2-ethyl-4,6-bis(benzhydryl)aniline, and light green is obtained after drying The powder (0.5g, 40.3%) is the Fe3 complex.

[0095] The structural confirmation data are as follows:

[0096] FT-IR (KBr, cm -1 ): 2871(w), 1630(m), 1596(ν C=N )(s), 1555(w), 1494(m), 1447(s), 1338(w), 1321(w), 1256(m), 1206(m), 1174(w), 1146(w), 1077(w), 1031(w), 1002(w), 969(w), 914(w), 850(w), 783(w), 743(w), 698(s)cm -1 .

[0097] Elemental Analysis: C 83 h 75 Cl 2 FeN 3 (1241.28) Theoretical: C, 80.31; H, 6.09; N, 3.39%. Experimental: C, 80.7; H, 5.08; N, 3.45%.

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Abstract

The invention provides a symmetrical seven-membered imino pyridine transition metal complex containing large steric hindrance substituent groups for preparing food-grade polyethylene wax, and a preparation method and application of the symmetrical seven-membered imino pyridine transition metal complex. The preparation method of the complex is mild in condition, short in cycle and easy to operate.The complex can be applied to a catalyst for ethylene polymerization, the catalytic activity center of the complex is single, the polymer molecular weight can be adjusted and controlled by changing aligand structure and polymerization conditions, and the complex has the advantages of low cost, high catalytic activity, good thermal stability and the like. Particularly, as for the provided iron complex, the maximum catalytic activity can reach 27.41*10<6> g.mol<-1>(Fe).h<-1>, even at 100 DEG C, 16.61*10<6> g.mol<-1>(Fe).h<-1> can be still kept, the operating temperature for industrial production is met, and great industrial application potential is achieved; and the obtained minimum polyethylene weight-average molecular weight Mw can reach 0.85 kg.mol<-1>, and the complex can be used for preparing the polyethylene wax in urgent need commercially, especially the food-grade wax, and has wide application prospects.

Description

technical field [0001] The invention relates to the technical field of polyolefin catalysts, in particular to a class of symmetrical seven-membered ring pyridine imine complexes containing large steric hindrance substituents that can be used to prepare low-molecular-weight polyethylene waxes, a preparation method and applications thereof. Background technique [0002] As a pillar product of modern science and technology and social development, polyolefin materials not only meet the needs of people's daily life in society, but also become indispensable and important materials in various fields such as cutting-edge technology and national defense construction. Among them, polyethylene (PE) is the most produced variety of general-purpose synthetic resins in the world. It has the characteristics of good chemical resistance, high mechanical strength, recyclability, and low cost. It occupies a pivotal position in the field of synthetic olefin materials. [0003] The design and dev...

Claims

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Application Information

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IPC IPC(8): C07F15/03C07F15/06C08F10/02C08F110/02C08F4/70
CPCC07F15/03C07F15/065C08F10/02C08F110/02C08F4/7042Y02P20/52
Inventor 孙文华巴里亚希尔·昌萨聂姆马艳平
Owner INST OF CHEM CHINESE ACAD OF SCI
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