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Nickel ethylene polymerization catalyzed system, preparation and use thereof

A technology of ethylene polymerization and catalyst, applied in the field of nickel ethylene polymerization catalyst components, which can solve the problems of complex catalyst synthesis steps and difficult preparation, and achieve the effects of easy purification, simple preparation route and high yield

Inactive Publication Date: 2006-09-13
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Wherein M is nickel, X is chlorine, bromine, iodine or alkyl, and the above-mentioned metal complex has a mononuclear structure, and the complex is used as a catalyst for olefin polymerization, and the obtained polymer has a unimodal molecular weight distribution, and the catalyst has a synthetic Weaknesses of complicated steps and difficult preparation

Method used

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  • Nickel ethylene polymerization catalyzed system, preparation and use thereof
  • Nickel ethylene polymerization catalyzed system, preparation and use thereof
  • Nickel ethylene polymerization catalyzed system, preparation and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Synthesis of ligand N, N'-(hydrogen-2-pyridine methylene)-3,3',5,5'-tetramethylbenzidine

[0042] Heat and dissolve 0.730g (3mmol) of 3,3',5,5'-tetramethylbenzidine in 10ml of absolute ethanol, add 0.810g (7.4mmol) of 2-pyridinecarbaldehyde dropwise under stirring, and heat to reflux for 10 hours , evaporated most of the solvent with a rotary evaporator, and recrystallized in absolute ethanol to obtain 1.116 g of bright yellow crystals, yield: 90%, m.p: 169-170 ° C. IR (cm -1 ): 3437 (NH), 1641 (C=N). EI-MS: m / z 418, 1 H NMR (CDCl 3): δ=8.74(d, 2H), 8.40(d, 2H), 8.32(d, 2H), 7.86(td, 2H), 7.43(td, 2H), 7.34(s, 4H), 2.25(s, 12H).Anal.For C 28 h 26 N 4 (%): calculated value C 80.35, H 6.26, N 13.39; experimental value C 80.34, H 6.36, N 13.37.

[0043] 2. Preparation of [N,N'-(hydrogen-2-pyridylmethylene)-3,3',5,5'-tetramethylbenzidine]nickel complex

[0044] 0.226g ligand N,N'-(hydrogen-2-pyridyl methylene)-3,3',5,5'-tetramethylbenzidine (0.5mmol) was heated an...

Embodiment 2

[0048] 1. The synthesis of ligand N, N'-(hydrogen-2-pyridine methylene)-3,3',5,5'-tetramethylbenzidine is the same as

[0049] Example 1.

[0050] 2. The preparation of [N, N'-(hydrogen-2-pyridine methylene)-3,3',5,5'-tetramethylbenzidine] nickel complex is the same as in Example 1.

[0051] 3. Polymerization of ethylene under normal pressure: At normal temperature and pressure, the dried 250 mL three-neck flask was evacuated and replaced with nitrogen three times, and the catalyst complex (3.4 mg, 5 μmol) was added under the protection of nitrogen. Replaced with ethylene gas three times. 50 mL of freshly distilled toluene and cocatalyst methylaluminoxane (MAO) (3.6 mL, 1.4 M, Al / Ni=500) were added in sequence, and an automatic gas supply device was used to maintain a constant pressure of ethylene during the reaction. After reacting for 60 minutes, 5% acidified ethanol was added to terminate the reaction. Add 200mL of absolute ethanol, shake, and precipitate the polymer pro...

Embodiment 3

[0054] 1. The synthesis of ligand N, N'-(hydrogen-2-pyridine methylene)-3,3',5,5'-tetramethylbenzidine: the same

[0055] Example 1.

[0056] 2. Preparation of [N, N'-(hydrogen-2-pyridylmethylene)-3,3',5,5'-tetramethylbenzidine] nickel complex: same as Example 1.

[0057] 3. Polymerization of ethylene under normal pressure: At normal temperature and pressure, the dried 250 mL three-neck flask was evacuated and replaced with nitrogen three times, and the catalyst complex (3.4 mg, 5 μmol) was added under the protection of nitrogen. Replaced with ethylene gas three times. Add 50 mL of freshly distilled toluene and cocatalyst methylaluminoxane (MAO) (5.8 mL, 1.4 M, Al / Ni=800) in sequence, and use an automatic gas supply device to maintain a constant pressure of ethylene during the reaction. After reacting for 60 minutes, 5% acidified ethanol was added to terminate the reaction. Add 200mL of absolute ethanol, shake, and precipitate the polymer product. After standing still for ...

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Abstract

This invention relates to a transition metal nickel catalyst component after ethylene polymerization. Component (A) is halogenated [N, N-(R bed -2-pyridine methylene)-substitution benzidine] nickel complexes, component (B) is alumina alkyl. The catalysis system is used to ethylene polymerization. There are high polymerization activity and high branching degree of complexes, and double peak feature of the complexes.

Description

technical field [0001] The present invention relates to a late transition metal nickel complex catalyst system for ethylene polymerization, in particular to a catalyst component containing N,N coordination for nickel ethylene polymerization, its preparation method, and its use in ethylene polymerization . Background technique: [0002] Polyolefin is the most important product in the modern petrochemical industry. Because of its excellent performance, it is widely used in various fields of the national economy and people's lives. Among them, polyethylene is one of the most important products and has become an independent branch of the petrochemical industry. In recent years, the research on late transition metal olefin polymerization and oligomerization catalysts has developed rapidly (Angew. Chem. Int. Ed. 1999, 38, 428-447; Chem. Rev. 2000, 100, 1169-1203). There is an urgent need to polymerize olefins through olefin polymerization catalysts with different structures to ob...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/02C08F4/80
Inventor 孙文华陈伟崔勇刘东兵邱波郑刚徐歆刘长城
Owner CHINA PETROLEUM & CHEM CORP