A kind of nickel base complex and its preparation method and application

A complex and nickel-based technology, which is applied in the direction of nickel organic compounds, can solve the problems of failing to meet the requirements of industrialization, poor thermal stability of catalysts, and rapid deactivation, etc., to achieve inhibition of aniline aromatic ring rotation, good temperature resistance, and increase in temperature. The effect of catalyst activity

Active Publication Date: 2018-03-16
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 1995, Brookhart et al. developed an α-diimine nickel and palladium catalyst to homogeneously catalyze ethylene polymerization to obtain high molecular weight branched polyethylene (J.Am.Chem.Soc. 1995, 117, 6414-6415), However, the thermal stability of the catalyst is poor, and when the polymerization temperature exceeds 35°C, it will rapidly deactivate, which is far from meeting the requirements of industrialization.

Method used

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  • A kind of nickel base complex and its preparation method and application
  • A kind of nickel base complex and its preparation method and application
  • A kind of nickel base complex and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Example 1 Synthesis of Ligand L1

[0059] Under nitrogen atmosphere and at room temperature, 100 mL of toluene, 2,6-di-tert-butyl-9,10-dihydro-9,10-ethylideneanthracene-11, 0.83 g (2.39 mmol) of 12-diketone, 0.975 g (0.96 mL, 5.5 mmol) of 2,6-diisopropylaniline, and a catalytic amount of p-toluenesulfonic acid were added, and heated at 110 °C to separate water and reflux for 24 hours . The reaction system gradually changed from light yellow to dark red, and released a lot of heat. The reacted mixture was rotary evaporated to remove the solvent, and the solid was recrystallized from ethanol to obtain a yellow solid powder with a yield of 75%. 1 H NMR (CDCl 3 , 300 MHz), δ (ppm): 1.03 (m, 12H), 1.5 (m, 12H), 1.23 (s, 18H), 2.53 (m, 4H), 4.91 (s, 2H), 7.07−7.25 (m , 12H). 13 C NMR (CDCl 3 , 400MHz), 22.30, 23.16, 28.28, 31.21, 34.79, 122.80, 123.91, 124.80, 135.31, 136.42, 138.46, 145.61, 150.29, 158.76.

Embodiment 2

[0060] Example 2 Synthesis of Ligand L2

[0061] According to the synthesis method of ligand L1 in Example 1, 2,6-dimethylaniline was used instead of 2,6-diisopropylaniline, and other operating conditions were the same. A tan solid powder was obtained, yield: 80%. 1 H NMR (CDCl 3 , 300 MHz), δ (ppm): 1.25(s, 18H), 1.82 (s, 6H), 1.91 (s, 6H), 3.49 (s, 2H), 6.99−7.23 (m, 12H).

Embodiment 3

[0062] Example 3 Synthesis of Ligand L3

[0063] According to the synthesis method of ligand L1 in Example 1, aniline was used instead of 2,6-diisopropylaniline, and other operating conditions were the same. A tan solid powder was obtained, yield: 85%. 1 H NMR (300MHz, CDC1 3 ), δ (ppm): 1.24 (s, 18H), 3.59 (s, 2H), 6.89−7.33 (m, 16H).

[0064] 2. Preparation of nickel-based complexes

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Abstract

The invention belongs to the field of catalytic polymerization of olefins, and specifically discloses a nickel-based complex, a preparation method and application thereof. The structural formula of the nickel-based complex is shown in formula (I), in which R1 and R2 are independently selected from hydrocarbon groups, aryl groups or aralkynyl groups, R3 is hydrogen or hydrocarbon groups, and X is halogen. The complex of the present invention has a large skeleton steric hindrance, can effectively inhibit the rotation of the aniline aromatic ring, effectively shield the metal center, increase its catalyst activity, and has good temperature resistance. It is suitable for industrial applications. Under the activation of different co-catalysts , can catalyze the polymerization of ethylene to obtain polyethylene with high molecular weight, narrow distribution, and high degree of branching; polymerize at a high temperature of 100°C to obtain polyethylene with a molecular weight of more than 105 g / mol, which has a good application prospect. Formula (I).

Description

technical field [0001] The invention belongs to the field of catalytic polymerization of olefins, and in particular relates to a nickel-based complex and its preparation method and application. Background technique [0002] Polyolefin is currently the most widely used polymer material in the world, and is widely used in industrial and agricultural production and daily life. In the early days, low-density polyethylene could only be synthesized through free radical polymerization under harsh conditions such as high temperature and high pressure; until the birth of Ziegler-Natta catalyst, high-density polyethylene was successfully synthesized through coordination polymerization. In 1995, Brookhart et al. developed an α-diimine nickel and palladium catalyst to homogeneously catalyze ethylene polymerization to obtain high molecular weight branched polyethylene (J.Am.Chem.Soc. 1995, 117, 6414-6415), However, the thermal stability of the catalyst is poor, and when the polymerizati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/04C08F110/02C08F4/70
Inventor 高海洋钟柳伍青
Owner SUN YAT SEN UNIV
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