Nickel base complex, and preparation method and application thereof

A complex, nickel-based technology, applied in the direction of nickel organic compounds, etc., can solve the problems of not meeting industrialization requirements, poor thermal stability of catalysts, rapid deactivation, etc. The effect of catalyst activity

Active Publication Date: 2016-02-03
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 catalyze ethylene polymerization in a homogeneous manner to obtain high molecular weight branched polyethylene (J.Am.Chem.Soc.1995, 117

Method used

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  • Nickel base complex, and preparation method and application thereof
  • Nickel base complex, and preparation method and application thereof
  • Nickel base complex, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] The synthesis of embodiment 1 ligand L1

[0059] Under nitrogen atmosphere and room temperature, add toluene 100mL, 2,6-di-tert-butyl-9,10-dihydro-9,10-ethylideneanthracene-11,12- Diketone 0.83g (2.39mmol), 2,6-diisopropylaniline 0.975g (0.96mL, 5.5mmol), and a catalytic amount of p-toluenesulfonic acid was added, 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 HNMR (CDCl 3 , 300MHz), 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 CNMR (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] The synthesis of embodiment 2 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 HNMR (CDCl 3 , 300MHz), 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] Synthesis of Example 3 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 HNMR (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 olefin catalytic polymerization, and particularly discloses a nickel base complex, and a preparation method and application thereof. The structural formula of the nickel base complex is as shown in a formula (I), wherein in the formula (I), R1 and R2 are independently selected from alkyl, aromatic base or arylenealkyne; R3 is hydrogen or alkyl; X is halogen. The complex provided by the invention has large skeleton steric hindrance, can effectively prevents an aniline aromatic ring from rotating, effectively shield a metal center, and increase the catalyst activity, is good in temperature resistance and applicable to industrial application, and can catalyze ethylene polymerization to obtain polyethylene with high molecular weight, narrow distribution and high branching coefficient under the activation of different cocatalysts; molecular weight of polyethylene obtained by polymerizing at high temperature of 100 DEG C reaches more than 105g/mol; the nickel base complex has better application prospect.

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 catalyze ethylene polymerization in a homogeneous manner 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 pol...

Claims

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Application Information

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