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Preparation method of nitrogen-doped carbon-supported monoatomic catalyst

A nitrogen-doped carbon and catalyst technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of complexity and cumbersome preparation process, and achieve simple operation and suitable for large-scale production Effect

Active Publication Date: 2019-07-12
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, atomic layer deposition and thermal emission technology require complex equipment, and the preparation process is cumbersome

Method used

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  • Preparation method of nitrogen-doped carbon-supported monoatomic catalyst
  • Preparation method of nitrogen-doped carbon-supported monoatomic catalyst
  • Preparation method of nitrogen-doped carbon-supported monoatomic catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step 1: Under stirring, dissolve copper acetate in deionized water to obtain a colored and transparent solution A with a concentration of 0.01mol / L, and then use a micro-injector to add the colored and transparent solution A drop by drop to the colored and transparent solution A with a volume of 5‰ The pyrrole monomer, continued magnetic stirring for 1h to obtain the reaction precursor;

[0026] Step 2: Transfer the reaction precursor to a polytetrafluoroethylene-lined stainless steel reactor with a filling ratio of 30% and conduct a hydrothermal reaction at 80°C for 5 hours. After the reaction, the product is centrifuged and then freeze-dried at -10°C ;

[0027] Step 3: Add the dried sample to an aqueous hydrochloric acid solution with a concentration of 1 mol / L, stir at room temperature for 1 hour to remove oxides, separate by suction filtration and wash, and then freeze-dry at -10°C;

[0028] Step 4: Put the sample dried in Step 3 in a porcelain boat, and heat it in...

Embodiment 2

[0030] Step 1: Under stirring, dissolve nickel acetate in deionized water to obtain a colored and transparent solution A with a concentration of 0.03mol / L, and then use a micro-injector to add the colored and transparent solution A drop by drop to the colored and transparent solution A with a volume of 10‰ The pyrrole monomer, continuous mechanical stirring for 8h to obtain the reaction precursor;

[0031] Step 2: Transfer the reaction precursor to a polytetrafluoroethylene-lined stainless steel reactor with a filling ratio of 40% and conduct a hydrothermal reaction at 100°C for 10 hours. After the reaction, the product is centrifuged and then freeze-dried at -80°C ;

[0032] Step 3: Add the dried sample to an aqueous hydrochloric acid solution with a concentration of 3 mol / L, stir at room temperature for 5 hours to remove oxides, separate by suction filtration and wash, then freeze-dry at -80°C;

[0033] Step 4: Place the sample dried in Step 3 in a porcelain boat, and heat ...

Embodiment 3

[0035] Step 1: Under stirring, dissolve cobalt acetate in deionized water to obtain a colored and transparent solution A with a concentration of 0.05mol / L, and then add the colored and transparent solution A to the colored and transparent solution A dropwise using a micro-injector with a volume of 8‰ The pyrrole monomer, continued magnetic stirring for 10h to obtain the reaction precursor;

[0036] Step 2: Transfer the reaction precursor to a polytetrafluoroethylene-lined stainless steel reactor at a filling ratio of 50% and conduct a hydrothermal reaction at 120°C for 12 hours. After the reaction, the product is centrifuged and then freeze-dried at -50°C ;

[0037] Step 3: Add the dried sample to an aqueous hydrochloric acid solution with a concentration of 5 mol / L, stir at room temperature for 10 h to remove oxides, separate and wash by suction, and then freeze-dry at -50°C;

[0038] Step 4: Place the sample dried in Step 3 in a porcelain boat, heat-treat in a tube furnace ...

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Abstract

The invention relates to a preparation method of a nitrogen-doped carbon-supported monoatomic catalyst. The method comprises the following steps of: dissolving transition metal acetate in deionized water, and adding a pyrrole monomer into the deionized water dropwise to obtain a reaction precursor; transferring the reaction precursor into a reaction kettle to carry out a hydrothermal reaction, andcarrying out centrifugal separation on the product and freeze drying the product after the reaction is finished; adding a dried sample into a hydrochloric acid solution to remove oxides, carrying outsuction filtration separation on the product, washing and freeze drying the product; and placing the dried sample into a porcelain boat, carrying out heat treatment in a tubular furnace in a protective atmosphere, and naturally cooling to obtain the nitrogen-doped carbon-supported monoatomic catalyst. Due to the existence of a ligand in the precursor complex, metal ions can be effectively prevented from being agglomerated to generate atomic clusters in the preparation process. Besides, the monoatomic loading capacity can be regulated by regulating parameters such as pyrrole, acid treatment time and the like. The method is green, efficient and easy to operate, no precise and complicated equipment is needed, and the method is suitable for large-scale production.

Description

technical field [0001] The invention relates to a preparation method of a single-atom catalyst, in particular to a preparation method of a nitrogen-doped carbon-supported single-atom catalyst. Background technique [0002] Compared with traditional macroscopic catalyst materials, single-atom catalysts have higher atom utilization efficiency and better catalytic effect, and have attracted widespread attention. The single atom itself acts as the active site and has intrinsic activity. After it is loaded on the carrier, it can have a strong interaction with the carrier. This effect can not only stabilize the single atom, but also regulate the electronic structure and improve the performance of the catalyst. . As a newly proposed class of catalysts, the preparation of single-atom catalysts is still an extremely challenging problem. Currently reported methods mainly include atomic layer deposition [Sun S, Zhang G, Gauquelin N, et al. Single-atom Catalysis Using Pt / Graphene Achi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/10B01J37/06B01J37/08
CPCB01J27/24B01J37/10B01J37/06B01J37/086
Inventor 曹丽云王勇黄剑锋寇领江李嘉胤
Owner SHAANXI UNIV OF SCI & TECH
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