Nitrogen-doped carbon-based metal monoatomic catalyst as well as preparation method and application thereof

A nitrogen-doped carbon, catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc. Avoid physical adsorption, improve catalytic activity, and increase the effect of loading

Inactive Publication Date: 2019-08-16
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problems that the carbon-based catalyst commonly used in the prior art is used to treat polluted water bodies, the reaction rate is slow, the catalyst activity is poor, the required dosage is large, and the catalyst stability is poor and cannot be reused. The invention provides a nitrogen-doped carbon-based metal single-atom catalyst and its preparation method and application

Method used

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  • Nitrogen-doped carbon-based metal monoatomic catalyst as well as preparation method and application thereof
  • Nitrogen-doped carbon-based metal monoatomic catalyst as well as preparation method and application thereof
  • Nitrogen-doped carbon-based metal monoatomic catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Step 1. Dissolve 1.0g (0.01mol) of calcium carbonate and 0.0483g (0.000179mol) of ferric chloride hexahydrate in 3ml of deionized water, let stand for 25min, and dry at 110°C for 9h to obtain FeCl 3 @CaCO 3 Precursor;

[0056] Step two, take 1.0g FeCl 3 @CaCO 3 Precursor, 2.7g 1,2-propylenediamine and 6.0g carbon tetrachloride were placed in a flask, ultrasonically dispersed for 5-10 minutes, refluxed at 70°C for 8h, and dried at 120°C for 10h;

[0057] Step 3, place the dried solid in a tube furnace, vacuumize, blow nitrogen, and carbonize at 600°C for 5 hours, with a heating rate of 5°C / min, to obtain a carbonized product;

[0058] Step 4: Wash the carbonized product with 1 mol / L HCl solution, wash with deionized water several times, and dry at 110°C for 8 hours to obtain the nitrogen-doped carbon-based metal single-atom catalyst (Fe-N-C catalyst).

[0059] The catalytic performance of the catalyst was evaluated by Fenton’s method of oxidation degradation of malac...

Embodiment 2

[0066] A preparation method of nitrogen-doped carbon-based metal single-atom catalyst:

[0067] Step 1. Dissolve 0.5g (0.005mol) of calcium carbonate and 0.049g (0.00018mol) of ferric chloride hexahydrate in 3ml of deionized water, let stand for 20min, and dry at 110°C for 9h to obtain FeCl 3 @CaCO 3 Precursor;

[0068] Step two, take 0.5g FeCl 3 @CaCO 3 Precursor, 2.5g 1,2-propanediamine and 5.0g carbon tetrachloride were placed in a flask, ultrasonically dispersed for 5-10 minutes, refluxed at 70°C for 8h, and dried at 120°C for 9h;

[0069] Step 3. Put the dried solid in a tube furnace, vacuumize, blow nitrogen, and carbonize at 400°C for 6 hours, with a heating rate of 3°C / min, to obtain a carbonized product;

[0070] Step 4: Wash the carbonized product with 2 mol / L HCl solution, wash with deionized water multiple times, and dry at 110° C. for 9 hours to obtain the nitrogen-doped carbon-based metal single-atom catalyst (Fe—N—C catalyst).

[0071] The transmission elec...

Embodiment 3

[0074] A preparation method of nitrogen-doped carbon-based metal single-atom catalyst:

[0075] Step 1. Dissolve 1.0g (0.01mol) of calcium carbonate and 0.049g (0.000103mol) of ferric chloride hexahydrate in 3ml of deionized water, let stand for 30min, and dry at 100°C for 10h to obtain FeCl 3 @CaCO 3 Precursor;

[0076] Step two, take 1.0g FeCl 3 @CaCO 3 Precursor, 1.7g 1,2-propylenediamine and 5.2g carbon tetrachloride were placed in a flask, ultrasonically dispersed for 5-10 minutes, refluxed at 70°C for 8h, and dried at 120°C for 8h;

[0077] Step 3, put the dried solid in a tube furnace, vacuumize, blow nitrogen, and carbonize at 800°C for 4 hours, with a heating rate of 10°C / min, to obtain a carbonized product;

[0078] Step 4: Wash the carbonized product with 3 mol / L HCl solution, wash with deionized water several times, and dry at 110° C. for 8 hours to obtain the nitrogen-doped carbon-based metal single-atom catalyst (Fe—N—C catalyst).

[0079] The transmission e...

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Abstract

The invention provides a nitrogen-doped carbon-based metal monoatomic catalyst as well as a preparation method and application thereof. A hard template method is selected to prepare the metal monoatomic catalyst, an amino-containing organic body and a chlorine-containing organic body are used as polymerization monomers, a transition metal salt is used as a metal source, a ratio relationship of a template, the organic monomers and the metal salt and reaction conditions are precisely regulated and controlled, so that in-situ polymerization of the organic monomers on the surface of the template and simultaneous chelating of transition metal ions can be realized to prepare the highly exposed monoatomic metal catalyst. The preparation method of the catalyst provided by the invention can ensurethe load capacity of the monoatomic metal to the greatest extent, and the condition that a nitrogen-doped carbon material wraps a metal oxide can be avoided through reasonable regulation and control of reparation conditions; and in addition, the Fenton catalyst prepared by the method has the advantages of high activity, a low metal loss rate and strong regeneration ability.

Description

technical field [0001] The invention relates to the technical field of material preparation, in particular to a nitrogen-doped carbon-based metal single-atom catalyst and its preparation method and application. Background technique [0002] Fenton oxidation technology is based on ferrous ion (Fe 2+ ) as a catalyst, hydrogen peroxide (H 2 o 2 ) Wastewater treatment method for chemical oxidation. The system composed of ferrous ions and hydrogen peroxide is also called Fenton's reagent, which can generate strong oxidative hydroxyl radicals, which can form organic free radicals with refractory organic substances in aqueous solution to destroy their structures and eventually oxidize and decompose. Fenton oxidation technology is widely used due to its simple operation and strong oxidation ability. However, the Fenton reaction has problems such as easy loss of iron ions, large amount of iron slag, low regeneration efficiency, and short service life of catalysts, which limit its ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10C02F1/72C02F101/38
CPCB01J27/24B01J35/1019B01J35/1038B01J35/1061C02F1/725C02F1/722C02F2305/026C02F2101/38
Inventor 牛建瑞丁鹏佳李再兴胡广志李卓然
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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