Preparation method of mesoporous carbon-based electrocatalyst

An electrocatalyst and mesoporous carbon technology, which is applied in the fields of carbon preparation/purification, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of long pre-carbonization time, low synthesis efficiency, and cumbersome synthesis process, etc. Achieve the effect of short preparation time, short time consumption and simple preparation process

Active Publication Date: 2020-12-04
GUANGZHOU UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The synthesis of mesoporous carbon materials often requires the addition of templates or template agents, and the template needs to be removed after synthesis. The synthesis process is cumbersome, time-consuming, and the synthesis efficiency is not high.
Moreover, mesoporous carbon materials generally need to be pre-carbonized (to prevent the material from rapidly decomposing due to excessive temperature rise, and ultimately fail to achieve the expected carbonization effect) and carbonization during the preparation process. The existing pre-carbonization process is relatively new. The material is calcined and pre-carbonized at a low temperature (≤500°C), the heating rate is slow, and the pre-carbonization time is long

Method used

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  • Preparation method of mesoporous carbon-based electrocatalyst
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  • Preparation method of mesoporous carbon-based electrocatalyst

Examples

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Embodiment 1

[0040] A method for preparing a mesoporous carbon-based electrocatalyst, comprising the following steps:

[0041] 1) Add the cysteine ​​solution (composed of cysteine ​​and water at a mass ratio of 1:8) dropwise to an equal mass of benzaldehyde solution (composed of benzaldehyde and ethanol at a mass ratio of 1:5), and heat Reflux at 120°C for 0.5h to obtain a reaction solution containing Schiff's base;

[0042] 2) Add nickel chloride solution (composed of nickel chloride and ethanol at a mass ratio of 1:8) dropwise to an equal mass of reaction solution containing Schiff base, stir evenly, and then heat to 120°C for distillation to obtain transition Metal Schiff base complexes;

[0043] 3) Place the transition metal Schiff base complex in an infrared drying oven for 20 minutes of infrared pre-carbonization, then place it in a tube furnace filled with nitrogen atmosphere, heat up to 700°C at a rate of 5°C / min, and carbonize for 2h, that is mesoporous carbon-based electrocatal...

Embodiment 2

[0045] A method for preparing a mesoporous carbon-based electrocatalyst, comprising the following steps:

[0046] 1) Arginine solution (composed of arginine and water at a mass ratio of 1:8) was added dropwise to 3 times the mass of salicylaldehyde solution (composed of salicylaldehyde and ethanol at a mass ratio of 1:7), Heating to 130°C for reflux reaction for 1 hour to obtain a reaction solution containing Schiff's base;

[0047] 2) Add cobalt nitrate solution (composed of cobalt nitrate and ethanol at a mass ratio of 1:12) dropwise to 0.5 times the mass of the reaction solution containing Schiff base, stir evenly, and then heat to 130°C for distillation to obtain transition metal Schiff base complexes;

[0048] 3) Place the transition metal Schiff base complex in an infrared drying oven for infrared pre-carbonization for 15 minutes, then place it in a tube furnace filled with nitrogen atmosphere, heat up to 800°C at a rate of 8°C / min, and carbonize for 0.5h. That is, the...

Embodiment 3

[0050] A method for preparing a mesoporous carbon-based electrocatalyst, comprising the following steps:

[0051] 1) Add thiourea solution (composed of thiourea and water at a mass ratio of 1:10) dropwise to twice the mass of vanillin solution (composed of vanillin and ethanol at a mass ratio of 1:10), and heat to 135°C Reflux reaction 1h, obtains the reaction solution containing Schiff's base;

[0052] 2) Add nickel nitrate solution (composed of nickel nitrate and ethanol at a mass ratio of 1:15) dropwise to an equal mass of reaction solution containing Schiff base, stir evenly, and then heat to 135°C for distillation to obtain a transition metal mat Phosphate base complexes;

[0053] 3) Place the transition metal Schiff base complex in an infrared drying oven for 30 minutes of infrared pre-carbonization, then place it in a tube furnace filled with nitrogen atmosphere, heat up to 750°C at a rate of 5°C / min, and carbonize for 1h, that is mesoporous carbon-based electrocataly...

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Abstract

The invention discloses a preparation method of a mesoporous carbon-based electrocatalyst. The preparation method comprises the following steps: 1) subjecting an amino compound to reacting with aromatic aldehyde to obtain Schiff base; 2) carrying out a reaction on the Schiff base and transition metal salt to obtain a transition metal Schiff base complex; and 3) carrying out infrared pre-carbonization and carbonization on the transition metal Schiff base complex to obtain the mesoporous carbon-based electrocatalyst. According to the method, a template agent does not need to be added, process issimple, consumed time is short, and the prepared mesoporous carbon-based electrocatalyst contains a large number of mesopores and is large in specific surface area, adjustable in types of active metal compounds and suitable for various electrocatalytic reactions.

Description

technical field [0001] The invention relates to the technical field of electrocatalysts, in particular to a preparation method of mesoporous carbon-based electrocatalysts. Background technique [0002] Mesoporous carbon materials are a new class of nanostructured materials, which have many advantages such as regular pore structure, high porosity, large specific surface area and pore volume, good thermal and chemical stability, etc. There are potential applications in many fields such as chemistry. The mesoporous structure of the mesoporous carbon material makes it have a high specific surface area, which is beneficial to the penetration of the electrolyte and the exposure of the catalytic active sites when used as an electrocatalyst, which can increase the electrocatalytic activity and the durability of the electrocatalyst. Therefore, mesoporous carbon-based electrocatalysts have become one of the research hotspots of electrocatalysis in the world. [0003] The synthesis o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/043B01J27/24B01J21/18B01J35/10C01B32/05C25B1/02C25B11/06
CPCB01J27/043B01J27/24B01J21/18B01J35/1023B01J35/1019B01J35/1061B01J35/0033C25B1/02C01B32/05C01P2002/72C01P2004/04Y02E60/50
Inventor 徐常威屈俊任
Owner GUANGZHOU UNIVERSITY
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