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Graphene oxide covalently immobilized metal phthalocyanine catalyst, preparation method and application thereof

A metal phthalocyanine and catalyst technology, which is applied in the field of graphene oxide supported photocatalysts, can solve the problems of affecting performance, weak stability of composite materials, weak binding force, etc., so as to improve firmness, improve conductivity, and improve dispersion sexual effect

Active Publication Date: 2019-03-29
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, iron phthalocyanine and graphene are mostly combined through physical interaction, and the binding force is weak, which leads to weak stability of the prepared composite material, thus affecting the performance of the composite material.

Method used

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  • Graphene oxide covalently immobilized metal phthalocyanine catalyst, preparation method and application thereof
  • Graphene oxide covalently immobilized metal phthalocyanine catalyst, preparation method and application thereof
  • Graphene oxide covalently immobilized metal phthalocyanine catalyst, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The first step, the preparation of (4-formylphenoxy) phthalonitrile: add 1.73 g (10 mmol) 4-nitrophthalonitrile, 2.44 g (20 mmol) p-hydroxy Benzaldehyde, 20 mL of solvent N-N dimethylformamide and 1.0 g of catalyst anhydrous K 2 CO 3 , keep the temperature at 80°C for 3 h, after the reaction is complete, pour the solution into an ice-water bath, let it stand still to precipitate a precipitate, filter it with suction, recrystallize from acetone, and dry it to obtain (4-formylphenoxy)phthalonitrile.

[0027] The second step, the preparation of tetra-β-(4-formylphenoxy) cobalt phthalocyanine: 0.496 g (2 mmol) (4-formylphenoxy) phthalonitrile and 0.26 g (2 mmol ) Anhydrous cobalt chloride was dissolved in 20 mL of n-amyl alcohol, heated to 90 °C, then 2 mL of DBU was added, and the temperature was raised to 140 °C for 24 h, and the reaction liquid was poured into 60 mL of ethanol and 180 mL of water (V:V=1 :3) in the mixed solution, let stand, and filter to obtain tetraki...

Embodiment 2

[0031] The first step, the preparation of (4-formylphenoxy) phthalonitrile: add 1.90 g (11 mmol) 4-nitrophthalonitrile, 2.56 g (21 mmol) p-hydroxy Benzaldehyde, 23 mL of solvent N-N dimethylformamide and 1.1 g of catalyst anhydrous K 2 CO 3 , constant temperature at 60°C for 4 h, after the reaction is complete, pour the solution into an ice-water bath, let it stand still to precipitate a precipitate, filter with suction, recrystallize from acetone, and dry to obtain (4-formylphenoxy)phthalonitrile.

[0032] The second step, the preparation of tetra-β-(4-formylphenoxy)iron phthalocyanine: 0.5346 g (2.2 mmol) (4-formylphenoxy) phthalonitrile and 0.38 g (2.2 mmol ) ferrous acetate was dissolved in 18 mL of n-amyl alcohol, heated to 100 °C, then added 2.16 mL of DBU, heated to 130 °C for 24 h, and the reaction solution was poured into 70 mL of ethanol and 210 mL of water (V:V=1: 3) in the mixed solution, stand still, and filter to obtain tetra-β-(4-formylphenoxy)iron phthalocyan...

Embodiment 3

[0036] The first step, the preparation of (4-formylphenoxy) phthalonitrile: add 0.21 g (12 mmol) 4-nitrophthalonitrile, 2.69 g (22 mmol) p-hydroxy Benzaldehyde, 24 mL of solvent N-N dimethylformamide and 1.2 g of catalyst anhydrous K 2 CO 3 , constant temperature at 80 ℃ for 5 h, after the reaction is complete, pour the solution into an ice-water bath, let it stand still to precipitate a precipitate, filter with suction, recrystallize from acetone, and dry to obtain (4-formylphenoxy)phthalonitrile.

[0037] The second step, the preparation of tetra-β-(4-formylphenoxy) manganese phthalocyanine: 0.5589 g (2.3 mmol) (4-formylphenoxy) phthalonitrile and 0.40 g (2.3 mmol ) Manganese acetate was dissolved in 19 mL of n-amyl alcohol, heated to 90 °C, then 2.25 mL of DBU was added, and the temperature was raised to 120 °C to react for 25 h, and the reaction liquid was poured into 80 mL of ethanol and 240 mL of water (V:V=1:3 ) in the mixed solution, let it stand, and filter to obtai...

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Abstract

The invention Belonging to the technical field of graphene oxide loaded photocatalysts, in order to solve the defects of easy aggregation, solubility in water, difficult separation and recovery and the like in phthalocyanine and polyoxometallate serving as a photocatalyst, the invention provides a graphene oxide covalently immobilized metal phthalocyanine catalyst, a preparation method and application thereof. Phthalocyanine and a derivative thereof are covalently bonded to modified graphene oxide to obtain a binary composite catalyst GO / Pc or GO / MPc; or phthalocyanine and a derivative as wellas polyoxometallate POM are loaded to modified graphene oxide together so as to obtain graphene oxide loaded phthalocyanine and POM ternary composite catalyst POM / GO / Pc or POM / GO / MPc. The method is conducive to separation and recovery of the catalyst, and at the same time avoids the easy aggregation defect of phthalocyanine. The graphene oxide covalently immobilized metal phthalocyanine catalystalso has a large specific surface area, expands the light response range, realizes the high catalytic activity of the composite ternary catalytic system under visible light, greatly improves the photoelectron-hole separation, and improves the photocatalytic activity.

Description

technical field [0001] The invention belongs to the technical field of graphene oxide-supported photocatalysts, and specifically relates to a graphene oxide-supported metal phthalocyanine catalyst and its preparation method and application. The graphene oxide-supported phthalocyanine catalyst is prepared by a covalent bonding method and Graphene oxide supported composite photocatalyst of phthalocyanine and polyoxometalates. Background technique [0002] Phthalocyanine compound is a kind of highly conjugated system with 18 π electrons, which has excellent catalytic performance, high chemical inertness and thermal stability, and excellent electron donating ability. The absorption of phthalocyanine is non-toxic and harmless to the environment, and it is cheap and easy to obtain. Therefore, it is a very promising visible light catalyst. , so that the photocatalytic activity is greatly reduced. Loading metal phthalocyanine on the carrier is one of the effective ways to avoid the...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J27/188B01J31/22B01J31/34C02F1/30C02F101/30C02F101/34C02F101/36
CPCB01J27/188B01J31/1625B01J31/183B01J31/34B01J2531/025B01J2531/16B01J2531/26B01J2531/72B01J2531/842B01J2531/845B01J2531/847C02F1/30C02F2101/308C02F2101/345C02F2101/36
Inventor 王蕊欣王立敏刘叶峰左鹏党利芳焦纬洲崔建兰
Owner ZHONGBEI UNIV
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