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Preparation and application of copper porphyrin catalyst and composite material thereof

A technology of composite materials and catalysts, applied in physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, organic chemistry, etc., can solve the problems of high cost of noble metals, consumption of electrolytes, high conversion voltage, etc., to achieve Fewer synthesis steps, easy separation, and reduced hydrogen evolution voltage

Active Publication Date: 2020-11-03
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The process of directly electrolyzing water to generate hydrogen requires high conversion voltage and consumes a large amount of electrolyte, which leads to high energy consumption and waste; platinum-based and other noble metal catalysts can greatly reduce the conversion voltage and electrolyte consumption of hydrogen production, but the cost of noble metals High cost and pollution to the environment

Method used

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  • Preparation and application of copper porphyrin catalyst and composite material thereof
  • Preparation and application of copper porphyrin catalyst and composite material thereof
  • Preparation and application of copper porphyrin catalyst and composite material thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] Embodiment 1 Synthetic bridged dialdehyde

[0089] This embodiment discloses a specific method for bridging dialdehydes: it specifically includes the following steps:

[0090] Step 1. Fully grind anhydrous potassium carbonate into powder, and bake at 200°C for 3 to 5 hours;

[0091] Step 2. Add powdered anhydrous potassium carbonate (20g, 145mmol) into N,N-dimethylformamide (80ml) under vigorous stirring, and keep the temperature at 60°C under the protection of inert gas;

[0092] Step 3, adding 5-tert-butyl salicylaldehyde (7.3g, 60.0mmol) for about 10 minutes;

[0093] Step 4, 1,3-dibromopropane (6.1g, 30mmol) was added to the reaction mixture, continued to stir for 12h, and tracked with a thin-layer chromatographic plate until the ratio of the product to the raw material no longer changed;

[0094] Step 5. Cool the reaction solution to -5°C, slowly add 100ml of water, and maintain the temperature of the reaction solution at 0 to 5°C while adding water;

[0095] St...

Embodiment 2

[0096] Embodiment 2 prepares wave type and saddle type copper porphyrin

[0097] This embodiment discloses the preparation method of 2-Cu-w and 2-Cu-s, which specifically includes the following steps:

[0098] Step 1, take carbon three bisaldehyde (3.8g, 10mmol), pyrrole (1.4mL, 20mmol) and Cu(OAc) 2 2H 2 O (3.6 g, 20 mmol) was added in portions to 200 mL of boiling propionic acid / butyric acid mixture (2:1, v / v); after reflux for 20 minutes, the air was isolated and stirring was continued for 45 minutes.

[0099] Step 2, removing the mixed acid by steaming under reduced pressure while it is hot;

[0100] Step 3, soak the solid residue in dichloromethane three times (80mL×3), combine the soaking solution, wash the solution five times with water, and dry it with anhydrous sodium sulfate;

[0101] Step 4, after distilling off the solvent, separate the first color band with dichloromethane / petroleum ether (1:4, v / v) by silica gel column chromatography, and use dichloromethane / p...

Embodiment 3

[0102] Embodiment 3 prepares wrinkled copper porphyrin

[0103] This embodiment discloses the preparation method of 1-Cu-r, which specifically includes the following steps:

[0104] Step 1, take carbon three dialdehyde white (3.8g, 10mmol), nitrophenyl bispyrromethane (5.3g, 20mmol) and Cu(OAc) 2 2H 2 O (3.6 g, 20 mmol) was added in portions to 200 mL of boiling propionic acid. After refluxing for 10 to 15 minutes, another equivalent of pyrrole (0.67 g, 10 mmol) was added to the mixed solution, and after 20 minutes of refluxing, the air was isolated and stirring was continued for 45 minutes;

[0105] Step 2, then remove propionic acid by steaming under reduced pressure while hot;

[0106] Step 3, the solid residue was soaked in dichloromethane three times (80 mL×3), the soaking solution was combined, the solution was washed with water five times, and dried over sodium sulfate.

[0107] Step 4, after removing the solvent, separate by silica gel column chromatography with dich...

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Abstract

The invention discloses a copper porphyrin catalyst, which has a structural formula shown in the specification, wherein a binding chain is a diether alkyl chain O(CH2)xO, and x is 2, 3, 4 or 5; or wherein the strapping chain is a diether alkyl chain O(CH2)xO, x is 2, 3, 4 or 5; or wherein the strapping chain is a diether alkyl chain O(CH2)xO, x is 3, 4, 5 or 6; the invention further discloses a compound formed by the compound and a carbon nano tube, a preparation method and application of the compound in the aspect of electrochemical hydrogen evolution catalysis. The compound has a non-planarstructure and good stability, and can be applied to electrochemical hydrogen evolution catalysis.

Description

technical field [0001] The invention relates to the technical field of electrochemical hydrogen evolution catalysts, in particular to the preparation and application of a copper porphyrin catalyst and a composite material formed with oxidized carbon nanotubes. Background technique [0002] Renewable energy refers to a kind of energy that can be continuously utilized and recycled in nature. With the emergence of the world's fossil energy crisis, people have realized the importance of renewable energy. Hydropower, wind power and other energies that have been vigorously developed in recent years come directly or indirectly from the conversion of solar energy and are renewable energy resources. However, the storage and transportation of these energies has become an insurmountable problem. The development of renewable energy sources with efficient energy storage technologies is crucial to address current energy and environmental challenges. Hydrogen is considered an ideal energy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22B01J31/22B01J21/18C25B11/06C25B1/04
CPCC07D487/22B01J31/183B01J31/1625B01J21/185C25B1/04C07B2200/13C07B2200/07B01J2531/16B01J2531/025B01J35/33Y02E60/36
Inventor 刘秋华周再春陈地龙林炳华
Owner HUNAN UNIV OF SCI & TECH
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