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A method for preparing metal-nitrogen-doped carbon catalytic materials using metal ionic liquids

A technology of nitrogen-doped carbon and catalytic materials, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc. High cost and other issues, to achieve good catalytic activity and selectivity, wide application range, and low cost effects

Active Publication Date: 2020-09-22
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Based on the concept of green chemistry, around CO 2 The electrochemical reduction reaction unfolds, making full use of CO 2 At the same time, it overcomes the shortcomings of the traditional M / C-X catalyst preparation process, such as cumbersome preparation process, high catalyst cost, and uneven distribution of catalyst components, and develops a set of green, safe and efficient preparation methods with very broad application prospects.

Method used

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  • A method for preparing metal-nitrogen-doped carbon catalytic materials using metal ionic liquids
  • A method for preparing metal-nitrogen-doped carbon catalytic materials using metal ionic liquids
  • A method for preparing metal-nitrogen-doped carbon catalytic materials using metal ionic liquids

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Experimental program
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Embodiment 1

[0040] The synthesis of embodiment 1, Ni / C-N material

[0041] The precursor used in the synthesis of Ni / C-N materials is a metal ionic liquid, the ionic liquid used is 1-butyl-3-methylimidazolium chloride [Bmim]Cl, and the nickel ion salt used is anhydrous NiCl 2 , the two are mixed and heated to obtain a metal ionic liquid [Bmim] 2 [NiCl 4 ], as shown in Formula II-1, and then the metal ionic liquid is pyrolyzed at high temperature to obtain Ni / C-N material. Specific steps are as follows:

[0042]

[0043] Add 1-butyl-3-methylimidazolium chloride salt and nickel chloride into a round bottom flask at a molar ratio of 1:1, stir at 70°C for 24 hours, and then perform multiple extractions with a small amount of dichloromethane Separation, and then use a vacuum rotary evaporator to rotate the extract at 50°C to remove dichloromethane and most of the water, and then place it in a vacuum drying oven to remove the remaining moisture. The drying temperature is 80°C. After dryi...

Embodiment 2

[0048] The synthesis of embodiment 2, Ni / C-N material

[0049] The precursor used in the synthesis of Ni / C-N materials is a metal ionic liquid, the ionic liquid used is 1-butyl-3-methylimidazolium bromide [Bmim]Br, and the nickel ion salt used is anhydrous NiBr 2 , the two are mixed and heated to obtain a metal ionic liquid [Bmim] 2 [NiBr 4 ], as shown in Formula II-2, and then the metal ionic liquid is pyrolyzed at high temperature to obtain Ni / C-N material. Specific steps are as follows:

[0050]

[0051] Add 1-butyl-3-methylimidazolium bromide and anhydrous nickel bromide into a round-bottomed flask at a molar ratio of 1:1, stir and react at 70°C for 24 hours, and then use a small amount of dichloromethane to Repeated extraction and separation, and then use a vacuum rotary evaporator to rotate the extract at 50°C to remove dichloromethane and most of the water, and then place it in a vacuum drying oven to remove the remaining moisture. The drying temperature is After...

Embodiment 3

[0054] The synthesis of embodiment 3, Ni / C-N material

[0055] The precursor used in the synthesis of Ni / C-N materials is a metal ionic liquid, the ionic liquid used is 1-butyl-3-methylimidazolium iodide [Bmim]I, and the nickel ion salt used is anhydrous NiI 2 , the two are mixed and heated to obtain a metal ionic liquid [Bmim] 2 [NiI 4 ], as shown in formula II-3, and then the metal ionic liquid is pyrolyzed at high temperature to obtain Ni / C-N material. Specific steps are as follows:

[0056]

[0057] Add 1-butyl-3-methylimidazolium iodide salt and anhydrous nickel iodide into a round-bottomed flask at a molar ratio of 1:1, stir and react at 70°C for 24 hours, and then use a small amount of dichloromethane to Repeated extraction and separation, and then use a vacuum rotary evaporator to rotate the extract at 50°C to remove dichloromethane and most of the water, and then place it in a vacuum drying oven to remove the remaining moisture. The drying temperature is After ...

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Abstract

The invention discloses a method for preparing metal-nitrogen-doped carbon catalytic materials using metal ionic liquid. The metal-nitrogen-doped carbon catalytic material is obtained by calcining a metal ionic liquid; the metal ionic liquid is obtained by a mixed reaction of an imidazole ionic liquid shown in Formula I and a bromide salt. The Ni / C-N material of the present invention can not only be used as CO 2 A good catalyst for electrocatalytic reduction reactions and is very effective in CO 2 Electroreduction to generate CO has good catalytic activity and selectivity. For example: 94% CO Faradaic efficiency at an overpotential of -0.75V (relative to a standard hydrogen electrode). Since the structure and properties of metal ionic liquids can be designed and regulated by changing anions and cations, the method of the present invention has the advantages of simplicity, convenience, low cost, adjustability, and wide application range, and can be applied to the synthesis of different types of M / C- N material.

Description

technical field [0001] The invention relates to a method for preparing a metal-nitrogen doped carbon catalytic material by using a metal ionic liquid, and belongs to the technical field of catalysts. Background technique [0002] Metal-carbon materials are regarded as the most promising catalysts due to their large specific surface area, low cost, unique physical and chemical properties, high utilization of surface atoms, and accessible reactants. Supporting heteroatoms (N, S, B, P, and halogen, etc.) in carbon materials can change the electronic environment and accelerate the transfer of protons and electrons in catalytic reactions. So far, researchers have focused on various M / C-X materials for highly efficient catalytic reactions. Generally, M / C-X materials are obtained by high-temperature pyrolysis of mixtures of carbon sources, metal sources, and heteroatom-containing compounds. This method is simple and convenient, and can be used to synthesize a variety of M / C-X mat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J35/10C25B1/00C25B11/06
CPCB01J27/24C25B1/00C25B11/091B01J35/399B01J35/393B01J35/23B01J35/33B01J35/613B01J35/633B01J35/647
Inventor 张建玲程修艳谭东兴谭秀娘石金彪杨冠英
Owner INST OF CHEM CHINESE ACAD OF SCI