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Post-transition metal catalyst system for oligomerization of ethylene

A post-transition metal and ethylene oligomerization technology, which is applied in the direction of physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problems of complex catalyst preparation and achieve convenient large-scale Mass production and storage, good water and oxygen resistance, good stability, and good reproducibility

Inactive Publication Date: 2003-11-05
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The catalysts developed by these patents generally have the characteristics of complex preparation

Method used

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  • Post-transition metal catalyst system for oligomerization of ethylene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Synthesis of ligand 4,5-diazafluorene-9-ketobenzoylhydrazone

[0024] Under the protection of nitrogen, dissolve 4,5-diazafluoren-9-one (0.911g, 5mmol) in absolute ethanol (25ml), add a catalytic amount of p-toluenesulfonic acid, heat slightly to reflux, and stir for 10 Add dropwise a solution of benzoyl hydrazide (0.681g, 5mmol) in absolute ethanol (15mml) within minutes, continue to reflux in absolute ethanol after dripping, stop the reaction after 8h, cool to precipitate a large amount of precipitate, filter with suction, and wash with ethanol. It was dried in vacuum to obtain 1.36 g of yellow solid, yield: 90%. EI-MS(m / z): 300(M + , 61.0%), 197 (15.7%), 181 (16.9%), 169 (13.7%), 154 (7.9%), 139 (3.6%), 122 (10.1%), 105 (100%), 94 (5.6 %), 77 (33.7%).

[0025] 2. Synthesis of 4,5-diazafluorene-9-ketobenzoylhydrazone nickel (II) complex catalyst precursor

[0026] Under the protection of nitrogen, dissolve 4,5-diazafluoren-9-one benzoyl hydrazone (0.060g, 0.2mmol) in a...

Embodiment 2

[0030] 1. Synthesis of ligand 4,5-diazafluoren-9-one-4-nitrobenzoylhydrazone:

[0031] Under the protection of nitrogen, dissolve 4,5-diazafluoren-9-one (0.911g, 5mmol) in absolute ethanol (25ml), add a catalytic amount of p-toluenesulfonic acid, heat slightly to reflux, and stir for 10 minutes Add 4-nitrobenzoyl hydrazide (0.906g, 5mmol) in anhydrous ethanol (25mml) solution dropwise, continue to reflux in anhydrous ethanol after dripping, stop the reaction after 8h, cool to precipitate a large amount of precipitate, filter with suction, It was washed with ethanol and dried in vacuum to obtain 1.59 g of yellow solid. Yield: 92%. IR(KBr): 3437, 3251, 3177, 3064, 3003, 1644(vs), 1592(s), 1566(m), 1517(s), 1400(s), 1337(vs), 1288, 1175, 1143 , 1097, 1009, 948, 861, 821, 756(m), 715(m); 1HNMR (DMSO): δ 7.50~7.65 (2H, m), 8.25 (4H, d), 8.4 (2H, d), 8.63 (1H, s), 8.80 (2H, d); FAB-MS (m / z): 344(M + -1); Anal.Calcd.for C 18 H 11 N 5 O 3 : C, 62.61%; H, 3.21%; N, 20.28%; O, 13.90%. Foun...

Embodiment 3

[0037] 1. Synthesis of ligand 4,5-diazafluorene-9-one-2-hydroxybenzoylhydrazone

[0038] Under the protection of nitrogen, dissolve 4,5-diazafluoren-9-one (0.911g, 5mmol) in absolute ethanol (25ml), add a catalytic amount of p-toluenesulfonic acid, heat slightly to reflux, and stir for 10 minutes Add 2-Hydroxybenzoic acid hydrazide (0.761g, 5mmol) in absolute ethanol (20mml) solution dropwise, continue to reflux in absolute ethanol after dripping, stop the reaction after 8h, cool to precipitate a large amount of precipitation, suction filter, ethanol Washing, vacuum drying, to obtain 1.34 g of light yellow solid, yield: 85%. IR(KBr): 3430(m), 3320(s), 3081(m), 2702, 2564, 1937, 1775, 1685(vs), 1604(s), 1565(s), 1519(vs), 1489( s), 1453(s), 1405(vs), 1365, 1282(s), 1234(m), 1201, 1162(m), 1132(s), 1107(s), 1060(m), 960, 894 , 753(vs); MALDI-TOF(m / z): 317(M + +1).

[0039] 2. Synthesis of catalyst precursor of 4,5-diazafluoren-9-one-2-hydroxybenzoylhydrazone nickel (II) complex:

[...

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Abstract

The catalyst is compound formed with 4, 5-diazefluorene-9-ketobenzoyl hydrazone and its derivative as ligand, NiCl2.6H2O and CoCl2. The catalyst is activated with cocatalyst MAO before used for catalyzing oligomerization of ethylene. The catalyst has high catalytic activity, is suitable for mass production and storage and has better industrial application foreground.

Description

Technical field [0001] The invention relates to an ethylene oligomerization catalyst system, in particular to a cobalt and nickel coordination catalyst of 4,5-diazafluoren-9-one benzoyl hydrazone and its derivatives, as well as a preparation method and an ethylene Application in Gathering. Background technique [0002] In recent years, the research of late transition metal complex catalysts for ethylene polymerization and oligomerization has been rapidly developed (Angew.Chem.Int.Ed., 1999, 38, 428~447; Chem. Rev., 2000, 100, 1169~1203), people strive to find new catalytic systems and improve existing catalytic systems in order to obtain high-activity and high-selectivity catalysts for olefin polymerization and oligomerization. Among the many catalytic systems, the nickel-based cationic catalytic system is a catalytic system that has been studied earlier and developed rapidly. Shell has developed SHOP based on US patents US Patent 3686351, 19727111 and US Pantent3676523, 19720822...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07C2/08
Inventor 孙文华陈立谊侯俊先朱宁李子龙胡友良李秀华
Owner INST OF CHEM CHINESE ACAD OF SCI
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