In-situ preparation method of zinc phthalocyanine/carbon nanotube composite catalyst based on solvothermal method

A carbon nanotube composite and carbon nanotube technology, which is applied in the field of material chemistry, can solve the problems of long reaction process time, troublesome post-processing, consumption of raw materials, etc., and achieve the effects of effective degradation, short reaction time, and easy post-processing.

Inactive Publication Date: 2015-10-07
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the prior art, the report on the carbon nanotube loading method basically adopts the impregnation method, but those skilled in the art know that the reaction process time of the ca

Method used

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  • In-situ preparation method of zinc phthalocyanine/carbon nanotube composite catalyst based on solvothermal method
  • In-situ preparation method of zinc phthalocyanine/carbon nanotube composite catalyst based on solvothermal method
  • In-situ preparation method of zinc phthalocyanine/carbon nanotube composite catalyst based on solvothermal method

Examples

Experimental program
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Embodiment 1

[0020] (1) Pretreatment of carbon nanotubes

[0021] Weigh 0.3029g of multi-walled carbon nanotubes, add 150mL of 65% concentrated nitric acid, heat and stir at 120°C for 9h, cool after the reaction, wash with water until neutral, and dry to obtain purified carbon nanotubes.

[0022] (2) Preparation of zinc phthalocyanine / carbon nanotube composites

[0023] Weigh 1.5mmol of zinc acetate dihydrate, 6mmol of phthalonitrile, 0.25g of carbon nanotubes and 0.2mL of 1,8-diazabicyclo[5,4,0]undec-7-ene (DBU) , add 50ml of absolute ethanol as a solvent, stir for 30 minutes and then pour it into the reaction kettle. After the reaction kettle is sealed, carry out solvothermal reaction at 190°C for 2 hours. After the reaction, stop heating and cool to room temperature naturally. The sample prepared above was taken out, and the remaining reactants adsorbed on the surface of the zinc phthalocyanine / carbon nanotubes were washed repeatedly with purified water and absolute ethanol, and then p...

Embodiment 2

[0025] (1) Pretreatment of carbon nanotubes

[0026] Weigh 0.5010g of multi-walled carbon nanotubes, add 150mL of 65% concentrated nitric acid, heat and stir at 120°C for 9h, cool after the reaction, wash with water until neutral, and dry to obtain purified carbon nanotubes.

[0027] (2) Preparation of zinc phthalocyanine / carbon nanotube composites

[0028] Weigh 1.5mmol of zinc acetate dihydrate, 6mmol of phthalonitrile, 0.4g of carbon nanotubes and 0.5mL of 1,8-diazabicyclo[5,4,0]undec-7-ene (DBU) , add 50ml of absolute ethanol as a solvent, stir for 30 minutes and then pour it into the reaction kettle. After the reaction kettle is sealed, carry out solvothermal reaction at 190°C for 4 hours. After the reaction, stop heating and cool to room temperature naturally. The sample prepared above was taken out, and the remaining reactants adsorbed on the surface of the zinc phthalocyanine / carbon nanotubes were washed repeatedly with purified water and absolute ethanol, and then pu...

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Abstract

The invention relates to an in-situ preparation method of a zinc phthalocyanine/carbon nanotube composite catalyst based on a solvothermal method. The in-situ preparation method comprises the steps of pretreating a carbon nanotube: adding concentrated nitric acid to the carbon nanotube, flowing back, heating, mixing, cooling, washing with water to be neutral, performing suction filtration, and drying; preparing the zinc phthalocyanine/carbon nanotube composite catalyst: adding the carbon nanotube, phthalonitrile, octan zinecnaty, 1,8-diazabicyclo [5,4,0] hendecane-7-alkene and the carbon nanotube to a beaker, adding a solvent, mixing for 30 minutes, and then pouring into a reaction still for solvothermal reaction. The in-situ preparation method has the beneficial effects that the used solvent is low in price and is easy to obtain, and no environmental pollution is generated; the preparation method of the zinc phthalocyanine/carbon nanotube is simple, the reaction time is short, the aftertreatment is easy, and industrial production is facilitated; effective degradation of pollutants malachite green is realized, and the photocatalytic activity is obviously better than that of pure zinc phthalocyanine particles.

Description

technical field [0001] The invention belongs to the technical field of material chemistry and relates to a method for preparing zinc phthalocyanine / carbon nanotube composite catalyst in situ based on a solvothermal method. Background technique [0002] Phthalocyanines, especially metal phthalocyanines, generally have good catalytic properties, because phthalocyanines have highly planar macrocyclic ligands, so that the catalytic reaction can occur in the axial position of the plane. At the same time, macrocyclic ligands not only have the properties of electron donors, but also have the characteristics of electron acceptors, so the ability of phthalocyanine to accept electrons can be adjusted by changing the metal element in the center of its skeleton and the substitution on the benzene ring around the ring. And the chemical properties of metal phthalocyanine are very stable. At present, many reactions including ammonia synthesis reaction, hydrogenation reaction, dehydrogenat...

Claims

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Application Information

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IPC IPC(8): B01J31/22
Inventor 李忠玉万毅陶玉瑶周亚文梁倩徐松
Owner CHANGZHOU UNIV
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