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Organic-inorganic composite nanometer photocatalyst and preparation method thereof

A nano-photocatalyst, inorganic composite technology, applied in organic compound/hydride/coordination complex catalysts, inorganic chemistry, chemical instruments and methods, etc., can solve the problem of poor solubility, unsatisfactory catalytic performance, and difficulty in uniform dispersion problem, to achieve the effect of improving solubility, improving solubility, and increasing dispersibility

Inactive Publication Date: 2020-05-22
YANGZHOU POLYTECHNIC INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the existing metal phthalocyanine has poor solubility due to its macromolecular conjugated system, so it is difficult to be uniformly dispersed in the catalytic system, and the catalytic performance of a single molybdenum disulfide as a photocatalyst is not ideal. Molybdenum disulfide material modified to improve catalytic efficiency

Method used

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  • Organic-inorganic composite nanometer photocatalyst and preparation method thereof
  • Organic-inorganic composite nanometer photocatalyst and preparation method thereof
  • Organic-inorganic composite nanometer photocatalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Preparation of Zinc Phthalocyanine

[0033] Under the protection of nitrogen, add 50 mL of dimethyl sulfoxide to the reaction flask, add 4 g of 4-nitrophthalonitrile and 7 g of p-hydroxybenzoic acid under stirring, then add 15 g of potassium carbonate, and stir at 30 ° C for 24 h , then add the reaction solution dropwise to 150mL of deionized water, adjust the pH value to 1 with concentrated hydrochloric acid, a flocculent precipitate precipitates, separate the precipitate by suction filtration, wash with deionized water, recrystallize with methanol, and then place at 50°C Dried in a vacuum oven to obtain 4-(4-carboxyphenoxy)phthalonitrile;

[0034] Under the protection of nitrogen, dissolve 2g of 4-(4-carboxyphenoxy)phthalonitrile and 0.8g of zinc chloride in 30mL of n-pentanol, heat up to 50°C and add 1,8-diazabicyclo Undec-7-ene 1.6mL, heated to 130°C and reacted for 6h, then cooled to room temperature, added hydrochloric acid to the reaction solution to adjust the ...

Embodiment 2

[0036] Preparation of cobalt phthalocyanine

[0037] Under the protection of nitrogen, add 50mL of dimethyl sulfoxide to the reaction flask, and add 3g of 4-nitrophthalonitrile and 7g of p-hydroxybenzoic acid under stirring, then add 12g of potassium carbonate, and stir at 30°C for 24h , then add the reaction solution dropwise to 150mL of deionized water, adjust the pH value to 1 with concentrated hydrochloric acid, a flocculent precipitate precipitates, separate the precipitate by suction filtration, wash with deionized water, recrystallize with methanol, and then place at 50°C Dried in a vacuum oven to obtain 4-(4-carboxyphenoxy)phthalonitrile;

[0038] Under the protection of nitrogen, dissolve 2g of 4-(4-carboxyphenoxy)phthalonitrile and 1g of cobalt acetate in 30mL of n-pentanol, and add 1,8-diazabicycloundecone after heating up to 50°C Carb-7-ene 1.6mL, heated to 130°C and reacted for 6h, cooled to room temperature, added hydrochloric acid to the reaction solution to ad...

Embodiment 3

[0040] Preparation of copper phthalocyanine

[0041] Under nitrogen protection, add 50 mL of dimethyl sulfoxide to the reaction flask, add 4 g of 3-nitrophthalonitrile and 7 g of p-hydroxybenzoic acid under stirring, then add 14 g of potassium carbonate, and stir for 24 hours at 30°C , then add the reaction solution dropwise to 150mL of deionized water, adjust the pH value to 1 with concentrated hydrochloric acid, a flocculent precipitate precipitates, separate the precipitate by suction filtration, wash with deionized water, recrystallize with methanol, and then place at 50°C Dried in a vacuum oven to obtain 4-(4-carboxyphenoxy)phthalonitrile;

[0042] Under nitrogen protection, dissolve 2 g of 4-(4-carboxyphenoxy)phthalonitrile and 0.7 g of cuprous chloride in 30 mL of n-pentanol, and add 1,8-diazabis Cycloundec-7-ene 1.6mL, heated to 130°C and reacted for 6h, cooled to room temperature, added hydrochloric acid to the reaction solution to adjust the pH to 1, a large amount ...

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Abstract

The invention discloses a preparation method for an organic-inorganic composite nanometer photocatalyst. According to the invention, with nitro-substituted phthalonitrile and p-hydroxybenzoic acid asraw materials, 4-carboxyl phenoxy substituted metal phthalocyanine is prepared through a two-step reaction, and metal phthalocyanine, graphene oxide and molybdenum disulfide are compounded to obtain ametal phthalocyanine, graphene and molybdenum disulfide ternary composite photocatalyst. According to the invention, p-carboxyl phenoxy is introduced onto a branched chain of the metal phthalocyanine, so the solubility of the metal phthalocyanine can be effectively improved, and the dispersion capability of the metal phthalocyanine serving as a photocatalyst in a reaction system is improved; themetal phthalocyanine, the graphene and the molybdenum disulfide are compounded to form the organic-inorganic composite nanometer photocatalyst, and through the synergistic effect of three components,the light absorption capacity is improved, and the light absorption range is widened; meanwhile, the active sites of the catalyst can be easily increased, and the catalytic activity is improved.

Description

technical field [0001] The invention relates to the technical field of photocatalysts, in particular to an organic-inorganic composite nano photocatalyst and a preparation method thereof. Background technique [0002] Phthalocyanine is a planar macrocyclic conjugated system composed of four isoindole units. The phthalocyanine molecule is a sixteen-membered ring composed of eight carbon atoms and eight nitrogen atoms alternately. It is a planar macrocycle with 18 π electrons. The π bond conjugated aromatic system has a very stable structure, and the length of each C-H bond is almost equal. At the same time, there is a hole in the phthalocyanine ring, which can accommodate various transition metal atoms such as cobalt, copper, iron, nickel, zinc, etc. These metal ions have a strong binding force with phthalocyanine, and their chemical properties are relatively stable. Metal phthalocyanines The compound has a strong transition in the visible light region and is easy to generat...

Claims

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Application Information

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IPC IPC(8): B01J31/34B01J31/22C01B3/04
CPCB01J31/34B01J31/184C01B3/042B01J35/39Y02E60/36
Inventor 黄德奇徐嘉琪王芳王雪源王元有
Owner YANGZHOU POLYTECHNIC INST
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