Preparation method of polycarbonate

A polycarbonate, copolymerization reaction technology, applied in the polymer field, can solve the problem of low catalytic activity

Active Publication Date: 2015-03-25
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the metalloporphyrin complexes disclosed in the prior art have relatively low catal

Method used

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  • Preparation method of polycarbonate

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[0027] The invention provides a kind of preparation method of polycarbonate, comprises the following steps:

[0028] Under the action of the main catalyst and the co-catalyst, the carbon dioxide and the epoxide are copolymerized to obtain polycarbonate;

[0029] The main catalyst is an aluminum porphyrin complex, and the aluminum porphyrin complex has a structure shown in formula I:

[0030] Formula I;

[0031] In formula I, the R 1 selected from halogen, aliphatic, substituted aliphatic, substituted heteroaliphatic, aryl, substituted aryl, or substituted heteroaryl;

[0032] The R 2 and R 3 independently selected from hydrogen, halogen, aliphatic, substituted aliphatic, substituted heteroaliphatic, aryl, substituted aryl, or substituted heteroaryl;

[0033] The Y is a halogen group, -NO 3 、CH 3 COO-, CCl 3 COO-, CF 3 COO-, ClO 4 -, BF 4 -, BPh 4 -, -CN, -N 3 , p-toluate, p-toluenesulfonate, o-nitrophenol oxyanion, p-nitrophenol oxyanion, m-nitrophenol oxyanion,...

Embodiment 1

[0110] at 25°C, N 2 Under protection, add 800mL dry dichloromethane, 2.8g 4-chlorobenzaldehyde (20mmol), 1.4mL pyrrole (20mmol) into a 1000mL round-bottomed three-neck flask, stir until the solid is completely dissolved, then add 3.7mL trifluoroacetic acid ( 50mmol, 2.5eq) and stirred for 1h, then added 9.08g DDQ (2.3-dichloro-5,6-dicyano-1,4-benzoquinone) and stirred for 1h. The above liquid was filtered under reduced pressure, the solvent was distilled off under reduced pressure, and the obtained crude product was separated by chromatographic column [stationary phase: aluminum oxide; mobile phase: dichloromethane / petroleum ether (volume ratio)=2:1] to obtain four (4-chlorophenyl) porphyrin, product conversion rate 20.8%; The present invention carries out proton nuclear magnetic resonance spectrum test to the tetrakis (4-chlorophenyl) porphyrin obtained, test result shows: 1 H NMR (300MHz, CDCl3), δ: 8.83(s, 8H), 8.12(d, J=9.0Hz, 8H), 7.78(d, J=9.0Hz, 8H), -2.87(s, 2H); iden...

Embodiment 2

[0114] at 25°C, N 2 Under protection, add 800mL of dry dichloromethane, 3.7g of 4-bromobenzaldehyde (20mmol), and 1.4mL of pyrrole (20mmol) into a 1000mL round-bottomed three-neck flask, stir until the solid is completely dissolved, then add 3.7mL of trifluoroacetic acid ( 50mmol, 2.5eq) and stirred for 1h, then added 9.08g DDQ (2.3-dichloro-5,6-dicyano-1,4-benzoquinone) and stirred for 1h. The above liquid was filtered under reduced pressure, the solvent was distilled off under reduced pressure, and the obtained crude product was separated by chromatographic column [stationary phase: aluminum oxide; mobile phase: dichloromethane / petroleum ether (volume ratio)=2:1] to obtain four (4-bromophenyl) porphyrin, product conversion rate 19.5%; The present invention carries out proton nuclear magnetic resonance spectrum test to the tetrakis (4-bromophenyl) porphyrin obtained, and test result is: 1 H NMR (300MHz, CDCl3), δ: 8.84 (s, 8H), 8.06 (d, J = 9.0Hz, 8H), 7.91 (d, J = 9.0Hz, 8H...

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Abstract

The invention provides a preparation method of polycarbonate. The method comprises the following step of performing copolymerization on carbon dioxide and epoxide under the effects of a main catalyst and a cocatalyst so as to obtain the polycarbonate, wherein the main catalyst has a formula I structure; the cocatalyst comprises one or a plurality of kinds of quaternary ammonium salt, quaternary microcosmic salt and organic alkali; the amount ratio of substances of the main catalyst to the substances of the cocatalyst is 1:(0.2-4). Compared with the prior art, by the preparation method, aluminum porphyrin compositions are adopted as the main catalyst, the electronic environment of aluminum in a metal active center is regulated by changing a substituent group, so that the electronic environment has a higher activity in the copolymerization of the carbon dioxide and the epoxide; in addition, the main catalyst has a higher product selectivity in the copolymerization, and the molecular weight of the obtained polycarbonate is higher. The experimental result indicates that the transforming amount of a catalytic system can be as high as 5563 h<-1> when the copolymerization of the carbon dioxide and the epoxide are catalyzed by the aluminum porphyrin compositions.

Description

technical field [0001] The invention belongs to the technical field of polymers, in particular to a preparation method of polycarbonate. Background technique [0002] Polycarbonate can be prepared by copolymerization of carbon dioxide and epoxide. Polycarbonate is a fully degradable polymer material with good transparency and excellent oxygen and water barrier properties. It is an ideal raw material for disposable packaging materials. , has wide application potential in food and medical packaging and other fields. [0003] Since Inoue realized the copolymerization of carbon dioxide and propylene oxide for the first time in 1969, alkyl zinc / active hydrogen catalytic systems, zinc carboxylate systems, double metal cyanide catalysts, rare earth three-way catalysts, diimine zinc catalysts, and tetradentate catalysts have successively appeared. A series of catalytic systems such as Schiff base cobalt complex catalytic system, zinc phenate catalytic system and metal porphyrin cat...

Claims

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Application Information

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IPC IPC(8): C08G64/34
Inventor 秦玉升郭洪辰王献红付双滨王佛松
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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