Preparation method of nitrogen-doped carbon-loaded metal monoatomic catalyst

A metal-loaded, nitrogen-doped carbon technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve the problems of high cost and complicated process, and achieve the method Simple, Inexpensive Effects

Inactive Publication Date: 2018-10-12
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the methods for preparing single-atom catalysts include coprecipitation, impregnation, atomic layer deposition, reverse Ostward (Ostward) ripening, stepwise reduction, and solid-phase melting. However, these methods have complex procedures and require acid Therefore, it is necessary to provide a simple and universal method for synthesizing single-atom catalysts

Method used

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  • Preparation method of nitrogen-doped carbon-loaded metal monoatomic catalyst
  • Preparation method of nitrogen-doped carbon-loaded metal monoatomic catalyst
  • Preparation method of nitrogen-doped carbon-loaded metal monoatomic catalyst

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[0031] The invention provides a method for preparing a nitrogen-doped carbon-supported metal single-atom catalyst, comprising the following steps:

[0032] (1) mixing soluble metal salt, hydroxylamine hydrochloride, soluble carbon source, water and ethanol to obtain a mixed solution;

[0033] (2) drying the mixed solution obtained in the step (1) to obtain a catalyst precursor;

[0034] (3) Calcining the catalyst precursor obtained in the step (2) to obtain a nitrogen-doped carbon-supported metal single-atom catalyst.

[0035] The invention mixes soluble metal salt, hydroxylamine hydrochloride, soluble carbon source, water and ethanol to obtain a mixed solution. In the present invention, the molar ratio of the soluble metal salt to hydroxylamine hydrochloride is preferably (0.001~0.01):(0.001~1), more preferably (0.002~0.008):(0.01~0.5), most preferably (0.004 ~0.006): (0.05~0.1).

[0036] In the present invention, the molar ratio of the soluble metal salt to the soluble ca...

Embodiment 1

[0049] Synthesis of W single-atom catalyst: using ammonium molybdate, hydroxylamine hydrochloride, and glucose as precursors, and synthesized through the steps of dissolution, precipitation, and calcination, the details are as follows:

[0050] (1) Weigh 0.0111 grams of ammonium tungstate and 0.69 grams of hydroxylamine hydrochloride into a beaker, add 40 milliliters of deionized water, and ultrasonically dissolve them for 5 minutes, then add 40 milliliters of alcohol, and then add 0.0544 grams of anhydrous glucose. After ultrasonically dissolving the mixture, it was dried in an oven at 70 °C.

[0051] (2) Take out the dried sample and put it in a porcelain boat, transfer it to a vacuum tube furnace, feed high-purity argon gas at a rate of 50 ml / min for protection, and turn the vacuum tube furnace at a speed of 5 degrees Celsius / min From room temperature to 600 degrees Celsius, keep warm for 4 hours.

[0052] (3) Cool down to room temperature in a vacuum tube furnace, take ou...

Embodiment 2

[0055] Synthesis of Mo single-atom catalyst: its synthesis steps are the same as W single-atom catalytic synthesis in Example 1, except that 0.0111 gram of ammonium tungstate is replaced by 0.0155 gram of ammonium molybdate, and the temperature of the vacuum tube furnace is changed to 650 degrees Celsius.

[0056] The nitrogen-doped carbon-supported metal single-atom catalyst prepared in this example is as figure 2 as shown, figure 2 a is the scanning transmission dark field image of Example 2, it can be seen that no obvious agglomerated particles appear, figure 2 b It can be seen that the Mo element is evenly distributed on the substrate, figure 2 c is an atomic resolution high-angle annular dark field image, it can be clearly seen that Mo single atoms are dispersed on the substrate, figure 2 In d, except for the X-ray diffraction peak of carbon element, there are no other crystal diffraction peaks. These results indicate that W element atoms are dispersedly distribute...

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Abstract

The invention provides a preparation method of a nitrogen-doped carbon-loaded metal monoatomic catalyst. The preparation method comprises the following steps: soluble metal salt, hydroxylamine hydrochloride, a soluble carbon source, water and ethanol are mixed to obtain a mixed solution, the mixed solution is subjected to drying precipitation to obtain a catalyst precursor, and the catalyst precursor is subjected to calcining to obtain the nitrogen-doped carbon-loaded metal monoatomic catalyst. According to the invention, metal salt, hydroxylamine hydrochloride, and the carbon source are fullymixed in the solution, the materials are dried and calcined, the carbon source is subjected to carbonization, ammonium ions are decomposed in nitrogen-doped carbon, the metal atoms are loaded at thenitrogen-doped carbon, the method is simple, and the cost is low.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a method for preparing a nitrogen-doped carbon-supported metal single-atom catalyst. Background technique [0002] The development of single-atom catalysts can maximize the catalytic efficiency of metals and reduce manufacturing costs. Theoretically speaking, the limit of dispersion of supported catalysts is that metals are evenly distributed on the support in the form of single atoms, which is not only the ideal state of supported metal catalysts, but also brings catalytic science to a smaller research scale— —Single atom catalysis. Single-atom catalysts are used in CO oxidation and selective oxidation, hydrogenation and selective hydrogenation, NO reduction and oxidation, water gas shift, organic synthesis, methanol steam reforming, fuel cells, photoelectric catalysis, formaldehyde oxidation, etc., so the preparation Single-atom metal catalysts have become an imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24
CPCB01J27/24B01J23/06B01J23/16B01J23/70B01J35/002B01J37/031B01J37/084B01J21/063B01J23/22B01J23/26B01J23/28B01J23/30B01J23/34B01J23/72B01J23/745B01J23/75B01J23/755B01J35/0013B01J37/0236B01J37/035B01J37/04
Inventor 韩丽丽刘熙俊罗俊
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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