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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 catalytic activity when they catalyze the copolymerization of carbon dioxide and epoxy compounds.

Method used

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  • Preparation method of polycarbonate

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preparation example Construction

[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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