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Preparation method of porphyrin aluminum complex and preparation method of polycarbonate

A technology of porphyrin complexes and ligand compounds, which is applied in the field of polymers and can solve problems such as inability to achieve high chemical structure selectivity

Inactive Publication Date: 2016-07-13
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the two-component aluminum-based porphyrin complexes disclosed in the prior art cannot achieve high chemical structure selectivity (>99%) when they catalyze the copolymerization of carbon dioxide and epoxides, resulting in highly alternating polycarbonates.

Method used

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  • Preparation method of porphyrin aluminum complex and preparation method of polycarbonate
  • Preparation method of porphyrin aluminum complex and preparation method of polycarbonate
  • Preparation method of porphyrin aluminum complex and preparation method of polycarbonate

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preparation example Construction

[0068] The preparation method of the aluminum-based porphyrin complex with the structure of formula (I) described in the application comprises the following steps:

[0069] A), under anhydrous and oxygen-free reaction conditions, compound A and pyrrole are dissolved in a solvent, and the first reaction is carried out under the action of a catalyst to obtain the first compound; the first compound is mixed with 2,3-dichloro- 5,6-dicyano-1,4-p-benzoquinone is subjected to a second reaction to obtain a second compound having a structure shown in formula (1);

[0070] The structural formula of the compound A is

[0071]

[0072] Wherein, R is selected from one of hydrogen, halogen, aliphatic group, substituted aliphatic group, aryl group or substituted aryl group.

[0073] B), the second compound obtained in A) and the metal salt compound are subjected to a third reaction in a solvent to obtain an aluminum-based porphyrin complex having a structure shown in formula (I); X in ...

Embodiment 1

[0133] Compound A (1,2,3,4,5,6,7,8-hydrogen-1:4,5:8-dimethylponthracene-9-carbaldehyde) used in this embodiment has a structure such as formula (17 ), R is hydrogen.

[0134]

[0135] (Step 1-1) Under anhydrous and anaerobic reaction conditions, 1.43g of compound A shown in formula (17) and 0.40g of pyrrole were dissolved in 600ml of dry dichloromethane solvent, followed by compound A and Add 1.2ml trifluoroacetic acid to the reaction solution of pyrrole, and carry out the first reaction at 25°C. After the first reaction time is 1h, add 3.5gDDQ to the obtained first reaction solution, and carry out the second reaction at 25°C , after the second reaction was carried out for 1 h, the obtained second reaction solution was spin-dried to obtain the crude product of the second compound, and then the crude product was purified by silica gel column chromatography to obtain a pure product, and the silica gel column The eluent used in the purification process was n-hexane and dichlo...

Embodiment 2

[0143] Compound A (1,2,3,4,5,6,7,8-Hydro-1:4,5:8-Dimethylpyronthracene-10-methoxy-9-carbaldehyde) used in this example , the structure is shown in formula (19), R is a methoxyl group.

[0144]

[0145] (Step 1-1) Under anhydrous and oxygen-free reaction conditions, 1.61 g of compound A shown in formula (19) and 0.40 g of pyrrole were dissolved in 600 ml of dry dichloromethane solvent, and then compound A and Add 1.2ml trifluoroacetic acid to the reaction solution of pyrrole, and carry out the first reaction at 25°C. After the first reaction time is 1h, add 3.5gDDQ to the obtained first reaction solution, and carry out the second reaction at 25°C , after the second reaction was carried out for 1 h, the obtained second reaction was vacuum removed to remove the solvent to obtain the crude product of the second compound, and then the crude product was purified by silica gel column chromatography to obtain a pure product, and the silica gel column The eluent used in the purific...

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Abstract

The invention provides a porphyrin aluminum complex with a structure as shown in a formula (I) or a formula (II), a preparation method of the porphyrin aluminum complex, and a preparation method of polycarbonate. Under the catalysis of a main catalyst and a cocatalyst of the porphyrin aluminum complex provided by the invention, carbon dioxide and epoxide are subjected to copolymerization, so that the polycarbonate is obtained. In a copolymerization process, the porphyrin aluminum complex participates in the reaction process and serves as the main catalyst, the porphyrin aluminum complex has high catalytic activity and particularly has excellent chemistry selectivity (which is greater than 99%), and the polycarbonate with low ether segments and high alternation is prepared.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to a preparation method of an aluminum-based porphyrin complex and polycarbonate. Background technique [0002] Since 1969, Professor Inoue in Japan used ZnEt for the first time 2 / H 2 O catalyzes CO 2 Since polycarbonate (PPC) was prepared by reacting with propylene oxide (PO), the preparation of polycarbonate has gradually attracted the attention of scientific researchers, and many efficient catalytic systems have been developed to catalyze the synthesis of carbon dioxide and epoxides. reaction. Polycarbonate is a polymer containing carbonate groups in its molecular chain. It is a fully degradable polymer material with good air permeability, oxygen and water barrier properties, and has been used in biodegradable pollution-free materials, new liquid crystal materials, gas barrier materials, reinforcing agents for rubber materials, composite materials and many other fields. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/06C08G64/34
CPCC07F5/069C08G64/34
Inventor 卓春伟秦玉升郭洪辰王献红王佛松
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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