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Preparation and application of a copper porphyrin catalyst and its composite material

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, high conversion voltage, consumption of electrolytes, etc., to achieve Fewer synthesis steps, mild conditions, and improved efficiency

Active Publication Date: 2021-08-31
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 a copper porphyrin catalyst and its composite material
  • Preparation and application of a copper porphyrin catalyst and its composite material
  • Preparation and application of a copper porphyrin catalyst and its composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] Example 1 Synthesis of bridged dialdehydes

[0089] The present embodiment discloses the concrete method of bridging dialdehyde: specifically comprises the following steps:

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

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

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

[0093] Step 4. Add 1,3-dibromopropane (6.1g, 30mmol) to the reaction mixture, continue stirring for 12h, and track with a thin-layer chromatographic plate until the ratio of the product to the raw material does not change;

[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 when adding water;

[0095] S...

Embodiment 2

[0096] Example 2 Preparation of wavy and saddle copper porphyrins

[0097] The present 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 dialdehyde (3.8g, 10mmol), pyrrole (1.4mL, 20mmol) and Cu(OAc) 2 ·2H 2 O (3.6 g, 20 mmol) was added portionwise to 200 mL of boiling propionic / butyric acid mixture (2:1, v / v); after 20 min at reflux, the air was shut off and stirring continued for 45 min.

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

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

[0101] Step 4. After the solvent is evaporated, the first color band is separated by silica gel column chromatography with dichloromethane / petroleum ether (1:4, v / v), and the first color band is separated with...

Embodiment 3

[0102] Example 3 Preparation of wrinkled copper porphyrin

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

[0104] Step 1, take carbon three bisaldehyde white (3.8g, 10mmol), nitrophenyl bispyrrole methane (5.3g, 20mmol) and Cu(OAc) 2 ·2H 2 O (3.6 g, 20 mmol) was added portionwise 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 the air was isolated after refluxing for 20 minutes, and stirring was continued for 45 minutes;

[0105] Step 2, then steam under pressure while still hot to remove propionic acid;

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

[0107] Step 4. After removing the solvent, separate with dichloromethane / petroleum e...

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Abstract

The invention discloses a copper porphyrin catalyst, the structural formula of which is: wherein the binding chain is a diether alkyl chain and is O(CH 2 ) x O, x is 2, 3, 4 or 5; or where the binding chain is a diether alkyl chain as O(CH 2 ) x O, x is 2, 3, 4 or 5; or where the binding chain is a diether alkyl chain as O(CH 2 ) x O, x is 3, 4, 5 or 6; the present invention also discloses the composite formed by the compound and carbon nanotubes and the preparation method and the application of the composite in electrochemical hydrogen evolution catalysis; the present invention has a non-planar structure, stable Well, the composite can be applied in 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 used and recycled in nature. With the emergence of the world's fossil energy crisis, people have realized the importance of renewable energy. Energy such as hydropower and wind power, which have been vigorously developed in recent years, are directly or indirectly derived from the conversion of solar energy and are renewable energy resources. However, the storage and transportation of these energy sources have become insurmountable problems. The development of renewable energy with efficient energy storage technologies is critical to addressing current energy and environmental challenges. Hydrogen is regarded as an ideal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22B01J31/22B01J21/18C25B11/095C25B1/04
CPCB01J21/185B01J31/1625B01J31/183B01J35/0033B01J2531/025B01J2531/16C07B2200/07C07B2200/13C07D487/22C25B1/04Y02E60/36
Inventor 刘秋华雷行周再春陈地龙林炳华
Owner HUNAN UNIV OF SCI & TECH
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