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Nickel complex and preparation and application thereof

A technology of metal complexes and nickel salts, which is applied in the field of nickel metal complexes and their preparation and application, and can solve the problems of difficult single catalysis of ethylene, increased process, and difficulty in improving the reactivity of ethylene, etc.

Inactive Publication Date: 2012-09-12
金永利 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the above catalyst research and development process, there are some problems: not only is it difficult to improve the reactivity of ethylene, but also it is difficult to obtain a single catalyst for ethylene oligomerization and polymerization.
In addition, the synthesis of nickel complex catalysts is completed in a multi-step synthesis process, which increases the number of procedures, and there is an urgent need for simple and convenient methods for preparing catalysts.

Method used

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  • Nickel complex and preparation and application thereof
  • Nickel complex and preparation and application thereof
  • Nickel complex and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] 1. Preparation of ligand: Preparation of 5,6,7-trihydroquinoline-8-ketal 2,6-diisopropylaniline [L3]: 5,6,7-trihydroquinoline-8- Ketone (0.59 g, 5 mmol) was mixed with 2,6-diisopropylaniline (0.6 g, 5.1 mmol) in an equimolar ratio, and a catalytic amount of p-toluenesulfonic acid (86 mg, 0.5 mmol) was added , Reflux reaction in 100 ml of toluene for 3h, the reaction must be carried out under the protection of nitrogen. At the same time, a water separator can be added to increase the yield. After the reaction is completed, the alumina column chromatography is separated to obtain a yellow oily ligand with a yield of 66%. FT-IR (KBr, cm -1 ): 3047, 2960, 2866, 2829, 1929.3, 1864, 1640 (v C = N), 1571, 1476, 1426, 1329, 1254, 1194, 1104, 1050, 1016, 796, 771, 674. 1 H NMR (400MHz, CDCl 3 ): δ 8.73 (d, J = 4.1 Hz, 1H, Py H); 7.57 (d, J = 7.7Hz, 1H, Py H); 7.30 (t, J = 4.5Hz, 1H, Py H); 7.14 ( d, J = 7.5 Hz, 2H, Ar H); 7.07 (t, J = 6.7 Hz, 1H, Ar H); 2.95 (t, J = 6.0 Hz, ...

Embodiment 2

[0047] 1. The preparation of catalyst Ni3 is the same as that in Example 1.

[0048] 2. Pressurized ethylene polymerization: heat the polymerization kettle to 100°C, evacuate while hot and replace with nitrogen for 3 times. Under the condition of pre-replacing the nitrogen in the kettle with ethylene, the polymerization kettle was allowed to cool down slowly to the expected polymerization temperature (20° C.). Rinse still three times with toluene, then add 50mL toluene successively, 20 mL is dissolved with the toluene solution of 1.5 μ mol catalyst (Ni3), 0.35mL promoter (EASC, the toluene solution of 0.43mol / L), described catalyst center metal nickel and promoter The molar ratio of metal aluminum in the catalyst is about 1:200, and toluene remains (so that the total amount of toluene is 100 ml). The kettle was closed, and ethylene was passed through to maintain a constant pressure of ethylene (10 atm). After the polymerization reaction reaches the preset time (30min), the e...

Embodiment 3

[0050] 1. The preparation of catalyst Ni3 is the same as that in Example 1.

[0051] 2. Pressurized ethylene polymerization: heat the polymerization kettle to 100°C, evacuate while hot and replace with nitrogen for 3 times. Under the condition of pre-replacing the nitrogen in the kettle with ethylene, the polymerization kettle was allowed to cool down slowly to the expected polymerization temperature (20° C.). Rinse the kettle three times with toluene, then add 50mL toluene successively, 20mL is dissolved with the toluene solution of 1.5μmol catalyst (Ni3), 0.41mL co-catalyst (AlEt 3 , 0.74mol / L toluene solution), the molar ratio of the metal nickel in the catalyst center to the metal aluminum in the cocatalyst is about 1:200, and the remaining toluene (making the total amount of toluene 100 milliliters). The kettle was closed, and ethylene was passed through to maintain a constant pressure of ethylene (10 atm). After the polymerization reaction reaches the preset time (30mi...

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Abstract

The invention discloses a nickel complex. The structure of the nickel complex is shown in the formula I, wherein R1 is C1-C3 alkyl; R2 is hydrogen, methyl or ethyl; R3 is hydrogen, halogen or aromatic base; and X is halogen. The invention also provides a preparation method and application of the nickel complex. The nickel complex has better catalytic property in the ethylene oligomerization and polymerization reactions in the presence of a cocatalyst aluminoxane or alkylaluminum. The polymerization activity of the complex reaches 1.24*10<7>g.mol<-1> (Ni).h<-1>, at the same time, the molecularweight distribution can be lowered to 1.8 and the oligomerization activity of the complex can reach 9.5*10<6>g.mol<-1> (Ni).h<-1>. The formula I is shown in the specification.

Description

technical field [0001] The invention relates to a nickel metal complex and its preparation and application. Background technique [0002] The rapid development of the ethylene oligomerization industry is largely due to the development of its catalyst and the huge application of α-olefin and polyethylene in today's life and industry. The method of a main industrial production linear alpha olefin is to apply SHOP type catalyst at present, and its structure is shown in the following formula (Angew.Chem., Int.Ed.Engl.1978,17,466-467; Angew.Chem., Int. Ed. Engl. 1983, 22, 503; J. Chem. Soc., Chem. Commun. 1994, 2203-2204): [0003] [0004] and Ziegler-Natta type catalysts (DE patent, 889229.1953-09-07; IT patent, 545332.1954; IT patent, 536899.1955; Belg patent, 533326.1955-05-05; Angew chem.1955, 67, 541-547; J Polym Sci PartA : Chem, 1955, 16: 143-154), Phillips type catalyst (Belg patent 530617.1955; US patent, 2825721.1958-03-04; Adv Catalysis, 1985, 33: 47-56) and meta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/04B01J31/22C07C2/32C07C11/08C08F110/02C08F4/70
Inventor 金永利曾艳宁余建刚
Owner 金永利
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