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Copper complex built by pyrimidine carboxylic acid base ligand, preparation method and use of copper complex

A copper complex, pyrimidine carboxylic acid technology, applied in copper organic compounds, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problem of poor polyphenylene ether selectivity, difficult catalyst recovery, solvent Environmental pollution and other problems, to achieve easy recovery, potential economic benefits, good selectivity

Active Publication Date: 2014-08-06
李建伟
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Problems solved by technology

[0009] In order to solve a series of problems such as poor selectivity, low yield, difficulty in catalyst recovery, and solvent pollution of the environment by oxidative coupling reaction of 2,6-dimethylphenol (DMP) to generate polyphenylene ether, the invention provides a method using N, O -Ligand 2,4-dihydroxypyrimidine-5-carboxylic acid and auxiliary ligand 2,2'-bipyridyl with Cu(ClO 4 ) 2 ·6H 2 O self-assembly reaction makes Cu (II) complex, also provides the method for preparing this complex, this complex can be used as catalyst for 2,6-xylenol (DMP) oxidative coupling reaction, prepares high yield, Highly Selective Polyphenylene Ether

Method used

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  • Copper complex built by pyrimidine carboxylic acid base ligand, preparation method and use of copper complex
  • Copper complex built by pyrimidine carboxylic acid base ligand, preparation method and use of copper complex
  • Copper complex built by pyrimidine carboxylic acid base ligand, preparation method and use of copper complex

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Embodiment 1

[0031] 15ml of 2,4-dihydroxypyrimidine-5-carboxylic acid and 2,2'-bipyridyl methanol solution (both 0.02mol·ml -3 ) was added dropwise to 4ml Cu(ClO 4 ) 2 ·6H 2 Aqueous solution of O (0.06mol·ml -3 ), shake well to obtain a blue clear solution, and after standing at room temperature for 3-5 days, a blue blocky crystal is obtained, namely, a pyrimidine carboxylate-based copper complex with a yield of 79%. After X-single crystal diffractometer analysis, it is a complex with mononuclear structure. Elemental analysis: according to the theoretical formula C 15 h 13 ClCuN 4 o 9 , Calculated: C 37.97, H 2.32, N 11.82%; Found: C 37.86, H 2.37, N 11.78%.

[0032] Used as a catalyst: at room temperature, add 2,6-dimethylphenol (122mg, 1mmol), sodium hydroxide (40mg, 1mmol), sodium dodecyl sulfate to a 10ml three-necked flask equipped with a condenser tube and a thermometer (SDS, 29 mg, 1 mmol), then add 5 mL of pure water, stir and add complex catalyst (0.02 mmol). Heat to 50°...

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Abstract

The invention relates to a copper complex, a preparation method of the copper complex, and a catalysis research result related to the copper complex. The copper complex has a mononuclear structure with the chemical formula of [Cu (dpca) (2,2'-bipy) (ClO4) (H2O)], wherein Hdpca=2,4-dyhydroxyl pyrimidine-5-carboxylic acid, and 2,2'-bipy=2, 2'-bipyridyl. The complex is formed by means of self-assembly cultivation of master ligand 2,4-dyhydroxyl pyrimidine-5-carboxylic acid, auxiliary ligand 2,2'-bipyridyl and Cu(ClO4)2.6H2O under room temperature, wherein the product has the characteristics of being high in stability, insoluble in water and most organic solvents, easy to separate, and reusable. The complex is taken as a catalyst to be used for the 2, 6-xylenol (DMP) oxidative coupling reaction, so that the polyphenyl ether (PPE) can be prepared with high selectivity, and a series of problems that the polyphenyl ether generated by the 2, 6-xylenol oxidative coupling reaction is bad in selectivity, low in yield, hard to recover catalyst, and capable of polluting the environment caused by the solvent can be solved.

Description

Technical field: [0001] The invention belongs to the technical field of metal-organic complex materials, and specifically relates to a copper complex constructed by pyrimidine carboxylic acid ligands and its preparation method and application. The copper complex has a mononuclear structure and exhibits excellent catalytic activity and selectivity. Background technique: [0002] The synthesis of metal-organic complexes by purposefully designing ligands and selecting metal ions has become one of the research hotspots in coordination chemistry today. This is not only due to the rich and colorful structures of organo-metallic complexes, but more importantly, they exhibit superior properties in many fields, such as optics, magnetism, adsorption separation, catalysis, and biological activity. The structure of the complex is affected by many factors, so it is difficult to predict the structure. Therefore, it is of great significance to systematically study the structure and proper...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F1/08B01J31/22C08G65/44
Inventor 肖博陈敏东
Owner 李建伟
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