Cyclopentadienyl transition metal nickel-nitrogen complex, as well as preparation method and applications thereof

A transition metal and complex technology, applied in the field of new catalytic material synthesis, achieves the effects of high yield, mild reaction conditions and good catalytic activity

Inactive Publication Date: 2014-07-30
HENGYANG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the stability and activity of such complexes need to be further improved.

Method used

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  • Cyclopentadienyl transition metal nickel-nitrogen complex, as well as preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Cyclocene transition metal nickel nitrogen complex 2{Ni 2 (C 10 h 8 N 2 ) 2 [C 8 h 10 (COO) 2 ] 2} 11H 2 The synthesis of O, its reaction steps are as follows:

[0029] Add 0.36mmol (0.0645g) of methylbicyclo[2.2.1]-2-heptene-5,6-dicarboxylic acid into a 50mL round bottom flask, add 10mL of a mixed solvent of DMF and water (volume ratio of 5:2 ) dissolved, stirred to dissolve, 0.48mmol (0.1262g) nickel sulfate hexahydrate was added to the above solution, heated and stirred, the temperature was controlled at 50°C, reacted for 3h, added 0.52mmol (0.0812g) 2,2'-linked Pyridine, the temperature is controlled at 50°C, the pH value is adjusted to 6-7, the reaction is stirred for 7 hours, the reaction solution is filtered while it is hot, and after the solution is cooled, filter, and the filtrate is covered with a layer of fresh-keeping film, and placed at room temperature to evaporate naturally, after 3 weeks Obtained blue crystals. The yield is about 46.4%. Eleme...

Embodiment 2

[0031] Cyclocene transition metal nickel nitrogen complex 2{Ni 2 (C 10 h 8 N 2 ) 2 [C 8 h 10 (COO) 2 ] 2} 11H 2 Synthesis of O:

[0032] 0.42mmol (0.0752g) of methylbicyclo[2.2.1]-2-heptene-5,6-dicarboxylic acid was added to a 50mL round bottom flask, and 12mL of a mixed solvent of DMAc, ethanol and water (volume ratio of 5 :1.5:1.5) dissolved, stirred to dissolve, 0.588mmol (0.0545g) nickel hydroxide was added to the above solution, heated and stirred, the temperature was controlled at 60°C, reacted for 2h, added 0.588mmol (0.0910g)2,2 '-Bipyridyl, the temperature is controlled at 60°C, the pH value is adjusted to 5-6, the reaction is stirred for 9 hours, the reaction solution is filtered while it is hot, and after the solution is cooled, it is filtered, and the filtrate is covered with a fresh-keeping film, and placed at room temperature to volatilize naturally, 3 After a week, blue crystals were obtained. The yield is about 47.3%.

Embodiment 3

[0034] Cyclocene transition metal nickel nitrogen complex 2{Ni 2 (C 10 h 8 N 2 ) 2 [C 8 h 10 (COO) 2 ] 2} 11H 2 Synthesis of O:

[0035] Add 0.48mmol (0.0752g) of methylbicyclo[2.2.1]-2-heptene-5,6-dicarboxylic acid into a 50mL round bottom flask, add 15mL of a mixed solvent of DMF and water (volume ratio of 7:2 ) was dissolved, stirred to dissolve, 0.94mmol (0.2232g) nickel acetate was added to the above solution, heated and stirred, the temperature was controlled at 65°C, reacted for 2h, and 0.672mmol (0.1048g) 2,2'-bipyridyl was added, Control the temperature at 65°C, adjust the pH value to 6-7, stir and react for 9 hours, filter the reaction solution while it is hot, and filter it after the solution is cooled. colored crystals. The yield is about 48.0%.

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Abstract

The invention discloses a cyclopentadienyl transition metal nickel-nitrogen complex, as well as a preparation method and applications thereof. The preparation method of the complex comprises the following steps: synthesizing raw materials, namely methyl bicyclo[2.2.1]-2-heptylene-5,6-phthalate, nickel salt, and 2,2'-bipyridyl by adopting a two-step method, and performing self-volatilization and crystallization to obtain 2{Ni2(C10H8N2)2[C8H10(COO)2]2}.11H2O crystals. The prepared nickel-nitrogen complex is stable in structure, has better catalytic activity on the esterification reaction, and is especially applicable to catalyzed synthesis of linear polyester resin.

Description

technical field [0001] The invention relates to a cyclocene-based transition metal nickel-nitrogen complex, a preparation method and an application thereof, and belongs to the field of synthesis of novel catalytic materials. Background technique [0002] In recent years, with the successful application of late transition metal complexes in olefin polymerization and atom transfer radical polymerization, the synthesis and catalytic performance of late transition metal nickel complexes have attracted great interest. At present, one of the research focuses on late-transition metal nickel complexes is to develop highly active and stable polymerization catalysts. A large number of existing research results show that the catalytic performance of organometallic compounds does not depend entirely on the central metal atom, but also depends on the coordination environment of the central metal, that is, the type, electron and space structure of the ligand. Therefore, the design and syn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/02C08G63/82C08G63/672
Inventor 李薇李昶红
Owner HENGYANG NORMAL UNIV
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