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Immobilization cationic metal porphyrin/heteropolyanion composite catalyst, preparation method and application method thereof

A heteropolyanion and composite catalyst technology, which is applied in the direction of organic compound/hydride/coordination complex catalysts, carbon-based compound preparation, chemical instruments and methods, etc., can solve difficult separation, inconvenient recycling, low catalytic activity and other problems, to achieve the effect of easy separation and recovery, good stability and high catalytic activity

Inactive Publication Date: 2015-07-01
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the invention of the present invention is to solve the shortcomings of existing cationic porphyrins such as poor chemical stability, low catalytic activity, difficulty in separation, and inconvenient recycling and use, and provide a highly catalytically active immobilized cationic metalloporphyrin / Heteropolyanion composite catalyst; and a preparation method of the polymer immobilized cationic porphyrin compound is provided

Method used

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  • Immobilization cationic metal porphyrin/heteropolyanion composite catalyst, preparation method and application method thereof
  • Immobilization cationic metal porphyrin/heteropolyanion composite catalyst, preparation method and application method thereof
  • Immobilization cationic metal porphyrin/heteropolyanion composite catalyst, preparation method and application method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: In a four-neck flask, add 1.0 g of cross-linked polystyrene microspheres ITMAPP-CPS immobilized with iodide-tris(p-trimethylammonium)phenylporphyrin and 40 mL of N,N-dimethylformamide , to fully swell the microspheres, then add 8.4mmol cobalt chloride, N 2 Under protection, react at 110°C for 4 hours, filter, wash repeatedly with distilled water and absolute ethanol, and dry in vacuum to obtain a dark brown solid catalyst CoP-CPS with cationic metalloporphyrin immobilized, and the immobilized amount of cationic cobalt porphyrin is 60 μmol / g.

[0022] Then in the four-necked flask, add 1.0g microspheres CoP-CPS and 20mL N,N-dimethylacetamide to fully swell the microspheres, and add phosphorus according to the molar ratio of CoP to phosphotungstic acid as 1: 1.2 Tungstic acid and 10 mL distilled water, N 2 Under protection, react at 40°C for 8 h, filter, wash with ethanol, and dry in vacuum to prepare the immobilized cationic metalloporphyrin / heteropolyani...

Embodiment 2

[0024] Example 2: In a four-neck flask, add 1.0 g of cross-linked polystyrene microspheres ITMAPP-CPS immobilized with iodide-tris(p-trimethylammonium)phenylporphyrin and 35 mL of N,N-dimethylacetamide , to fully swell the microspheres, then add 8 mmol ferric chloride, N 2 Under protection, react at 100°C for 3 hours, filter, wash repeatedly with distilled water and absolute ethanol, and dry in vacuum to obtain a dark brown solid catalyst FeP-CPS with cationic metalloporphyrin immobilized, and the immobilized amount of cationic iron porphyrin is 51 μmol / g.

[0025] Then in the four-neck flask, add 1.0g microspheres FeP-CPS and 20mL dimethyl sulfoxide to fully swell the microspheres, add phosphotungstic acid and 8mL Distilled water, N 2 Under protection, react at 45°C for 7 h, filter, wash with ethanol, and dry in vacuum to prepare the immobilized cationic metalloporphyrin / heteropolyanion composite catalyst FePPW-CPS.

[0026] In the reactor, add 20ml ethylbenzene and 0.3...

Embodiment 3

[0027] Example 3: In a four-neck flask, add 1.0 g of cross-linked polystyrene microspheres ITMAPP-CPS immobilized with iodide-tri(p-trimethylammonium)phenylporphyrin and 45 mL of dimethyl sulfoxide to make the microspheres Fully swell, then add 9 mmol manganese chloride, N 2 Under protection, react at 105°C for 2 hours, filter, wash repeatedly with distilled water and absolute ethanol, and dry in vacuum to obtain a dark brown solid catalyst MnP-CPS immobilized with cationic metalloporphyrin, and the immobilized amount of cationic manganese porphyrin is 53 μmol / g.

[0028] Then in the four-necked flask, add 1.0g microspheres MnP-CPS and 20mL N,N-dimethylformamide to fully swell the microspheres, and add phosphorus in a ratio of 1:1 by the molar ratio of MnP to phosphomolybdic acid molybdic acid and 9 mL distilled water, N 2 Under protection, react at 35°C for 7 h, filter, wash with ethanol, and dry in vacuum to prepare the immobilized cationic metalloporphyrin / heteropolyan...

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Abstract

The invention belongs to the technical field of heterogeneous phase catalysis, specifically to an immobilization cationic metal porphyrin / heteropolyanion composite catalyst, a preparation method and an application method thereof. With the present invention, disadvantages of poor chemical stability, low catalysis activity, difficult separation, inconvenient recycling and the like of the existing cationic porphyrin are solved. According to the preparation method, a complex reaction of the immobilization cationic phenyl porphyrin and a metal salt is adopted to prepare the immobilization cationic metal porphyrin; base on the previous process, a heteropolyacid is adopted as a reagent, and a static electricity interaction effect of the cationic metal porphyrin and the heteropolyanion is adopted to prepare the immobilization cationic metal porphyrin / heteropolyanion composite catalyst. According to the present invention, in the structure components of the composite catalyst, the heteropolyanion can effectively protect cobalt porphyrin to prevent the cobalt porphyrin from oxidative inactivation, such that the catalyst can maintain stable high catalysis activity and has a good recycle performance.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalysis, and specifically relates to a solid-supported cationic metal porphyrin / heteropolyanion composite catalyst and a preparation and application method thereof. Background technique [0002] Metalloporphyrin catalysts have good catalytic activity in the oxidation process of hydrocarbons. Among metalloporphyrin (MPs) biomimetic catalysts, cationic metalloporphyrin is an important type, which has been widely used in the catalytic oxidation process of hydrocarbons. However, at present, cationic metalloporphyrins are mostly used in the form of small molecules, which have disadvantages such as poor chemical stability, difficult separation, and inconvenient recycling. Since the molecular structure of the cationic metalloporphyrin contains multiple cationic groups, it provides sufficient conditions for the immobilization of the cationic metalloporphyrin and other stabilizing modifications. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/34C07C49/78C07C45/36
CPCY02P20/584
Inventor 王蕊欣王洪静高保娇门吉英李延斌顾来沅喻龙
Owner ZHONGBEI UNIV
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