Copper-nitrogen co-doped carbon nanotube catalyst and preparation method and application thereof

A carbon nanotube and co-doping technology, which is applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc. High reducing activity, easy to control, easy to control the effect of loading

Inactive Publication Date: 2018-06-22
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These preparation methods have high equipment requirements, complicated preparation process, and uncontrollable nitrogen doping amount.

Method used

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  • Copper-nitrogen co-doped carbon nanotube catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Take a certain amount of commercial carbon nanotubes with a diameter of 10-20nm, in 30% HNO 3 Reflux at 80°C for 3 hours, rinse with deionized water until neutral after cooling, and dry. Dissolve the dried carbon nanotubes in 0.01mol / L Cu(NO 3 ) 2 In the aqueous solution, the mass ratio of copper to carbon nanotubes is 1:100. Add 0.01mol / L citric acid, place it on a magnetic stirrer and stir continuously, and slowly add NaOH solution during the stirring process to adjust the pH of the solution to neutral. The suspension obtained by the above stirring was ultrasonically dispersed at 5°C for 2 hours, continued to stir for 24 hours, and then was taken out and dried. The obtained powder was roasted in nitrogen, the gas flow rate of the nitrogen atmosphere was 100mL / min, the temperature was raised from room temperature to 350°C at a rate of 10°C / min, and the temperature was kept for 5h. After cooling down to room temperature, pass H 2 atmosphere for reduction, H 2 The ...

Embodiment 2

[0056] Take a certain amount of commercial carbon nanotubes with a diameter of 10-20nm, in 30% HNO 3 Reflux at 80°C for 3 hours, rinse with deionized water until neutral after cooling, and dry. Dissolve the dried carbon nanotubes in 0.01mol / L Cu(NO 3 ) 2 In the aqueous solution, the mass ratio of copper to carbon nanotubes is 1:50. Add 0.01mol / L sodium citrate, place it on a magnetic stirrer and stir continuously, and slowly add NaOH solution during the stirring process to adjust the pH of the solution to neutral. The suspension obtained by the above stirring was ultrasonically dispersed at 5°C for 2 hours, continued to stir for 24 hours, and then was taken out and dried. The obtained powder was roasted in nitrogen, the gas flow rate of the nitrogen atmosphere was 100mL / min, the temperature was raised from room temperature to 350°C at a rate of 10°C / min, and the temperature was kept for 5h. After cooling down to room temperature, pass H 2 atmosphere for reduction, H 2 Th...

Embodiment 3

[0058] Take a certain amount of commercial carbon nanotubes with a diameter of 10-20nm, in 30% HNO 3 Reflux at 80°C for 3 hours, rinse with deionized water until neutral after cooling, and dry. Dissolve the dried carbon nanotubes in 0.01mol / L Cu(NO 3 ) 2 In the aqueous solution, the mass ratio of copper to carbon nanotubes is 1:20. Add 0.01mol / L citric acid, place it on a magnetic stirrer and stir continuously, and slowly add NaOH solution during the stirring process to adjust the pH of the solution to neutral. The suspension obtained by the above stirring was ultrasonically dispersed at 5° C. for 2 h, continued stirring for 24 h, and then taken out and dried. The obtained powder was roasted in nitrogen, the gas flow rate of the nitrogen atmosphere was 100mL / min, the temperature was raised from room temperature to 350°C at a rate of 10°C / min, and the temperature was kept for 5h. After cooling down to room temperature, pass H 2 atmosphere for reduction, H 2 The gas flow r...

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Abstract

The invention provides a copper-nitrogen co-doped carbon nanotube catalyst and a preparation method and application thereof. The preparation method comprises the following steps of: (1) adopting carbon nanotubes as a substrate, performing reflux in an acidic solution, performing washing with water until neutrality is achieved, and performing drying; (2) adding a copper salt solution and dispersantinto the carbon nanotube powder obtained in the step (1), performing stirring, and adding a pH adjusting agent until a neutral state is achieved during stirring; (3) performing ultrasonic dispersionon the suspension obtained in the step (2), then performing stirring, and carrying out drying; (4) calcining the dried powder in the step (3) successively in an inert gas atmosphere and a reducing gasatmosphere so as to obtain copper-doped carbon nanotubes; (5) transferring the copper-doped carbon nanotubes obtained in the step (4) to a hydrothermal reaction kettle, adding a nitrogen source, andperforming a reaction; and (6) washing the suspension obtained in the step (5) to neutral, and performing drying. The preparation method has low cost, and is simple and easy to control, and the catalyst has high reduction activity in an electrocatalytic process of CO2.

Description

technical field [0001] The invention relates to a copper-nitrogen co-doped carbon nanotube catalyst and its preparation method and application, belonging to the field of inorganic nano-catalytic materials. Background technique [0002] With the development of human society, a series of energy activities have intensified, and CO in the atmosphere 2 content is continuously increasing. CO 2 As the most important greenhouse gas, the global warming and ecological problems caused by it are severe challenges to the sustainable development of human beings. CO 2 The recycling conversion is to reduce CO 2 One of the important ways of content. Traditional conversion methods such as CO 2 Hydrogenation or catalytic reforming with natural gas to produce synthesis gas, etc., are usually carried out under high temperature and pressure. In comparison, the electrochemical reduction principle is CO 2 Conversion provides a milder means of recycling, and its reaction rate and product sele...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/34B01J37/08B01J37/10B01J37/16B01D53/86B01D53/62
CPCB01D53/864B01J27/24B01J35/0033B01J37/082B01J37/088B01J37/10B01J37/16B01J37/343Y02A50/20
Inventor 张佳舟陈为魏伟孙予罕
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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