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A nitrogen-containing amorphous carbon layer-wrapped carbon nanotube one-dimensional material with a core-shell structure and its preparation method and application

A technology of carbon nanotubes and amorphous carbon, applied in nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problems of low methanol resistance, high price, poor stability, etc., and achieve high temperature treatment The effect of short time, high safety and good stability

Inactive Publication Date: 2017-06-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method of the present invention can effectively overcome the defects of the existing catalysts, which are expensive due to the use of noble metals, and have low methanol resistance and poor stability.

Method used

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  • A nitrogen-containing amorphous carbon layer-wrapped carbon nanotube one-dimensional material with a core-shell structure and its preparation method and application
  • A nitrogen-containing amorphous carbon layer-wrapped carbon nanotube one-dimensional material with a core-shell structure and its preparation method and application
  • A nitrogen-containing amorphous carbon layer-wrapped carbon nanotube one-dimensional material with a core-shell structure and its preparation method and application

Examples

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Effect test

Embodiment 1

[0044] Disperse 200 mg of carboxylated carbon nanotubes in 2 mL of DMF and 40 mL of SOCl 2 In the mixed solution, the temperature was raised to 65 degrees Celsius and stirred for 24 hours, then centrifuged and dried. Ultrasonic dispersion of the above obtained product in 50 mL THF, adding 500 mg of p-phenylenediamine and refluxing for 24 hours, the obtained product was centrifuged and dried to obtain amino carbon nanotubes. Prepare ethanol solution 1 dissolved with terephthalaldehyde (4mg / mL) and acetic acid, and ethanol solution dissolved with 5, 10, 15, 20-tetrakis(4-aminophenyl) porphyrin (6mg / mL) and acetic acid Solution 2. Under ultrasonic conditions, ultrasonically disperse the amino-modified carbon nanotubes in solution 1 and keep ultrasonic for 30 min, then centrifuge; under ultrasonic conditions, ultrasonically disperse the material obtained by centrifugation in solution 2 and keep ultrasonic for 30 min, then centrifuge ; Repeat the above operation once, and heat an...

Embodiment 2

[0046] The preparation process of Example 1 is adopted, except that the amount of iron metal salt used is increased to 20-50 mg. Depend on Figure 4 It is known that the material obtained under this condition can observe iron nitride species through XRD characterization, and at the same time by image 3 Metal particles can also be clearly observed in TEM photographs. Its oxygen reduction reaction activity is shown in Figure 5 , the limiting diffusion current can reach 5.7mA / cm 2 , the half-wave potential is about -0.15V.

Embodiment 3

[0048] The preparation process of Example 2 is adopted, except that the amount of iron metal salt used is increased to 50-80 mg. Depend on Figure 4 It is known that the material obtained under this condition can observe iron nitride and ferric oxide species through XRD characterization, and at the same time, metal particles can also be clearly observed on the TEM photo. Its redox reaction activity can be seen in Figure 5 , the limiting diffusion current can reach 5.0mA / cm 2 , the half-wave potential is about -0.2V.

[0049] The invention relates to a nitrogen-containing amorphous carbon layer-wrapped carbon nanotube oxygen reduction catalyst with a core-shell structure, a preparation method and application thereof. Specifically, the surface of carbon nanotubes is coated with a layer of porphyrin formed by the reaction of terephthalaldehyde and 5, 10, 15, 20-tetrakis (4-aminophenyl) porphyrin monomers through the condensation reaction of amino-aldehyde groups. polymer. A...

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Abstract

The invention relates to a nitrogen-containing amorphous carbon layer-wrapped carbon nanotube oxygen reduction catalyst with a core-shell structure. The specific preparation steps are as follows: at room temperature, appropriate amounts of terephthalaldehyde and tetrakis(4-carboxyphenyl)porphyrin are respectively dissolved in ethanol solution, and then a certain amount of acetic acid solution is added to the two solutions respectively. Then ultrasonically disperse the amino-modified carbon nanotubes in the terephthalaldehyde solution and keep ultrasonicating for a period of time. Next, the carbon nanotubes are separated by centrifugation, and then these carbon nanotubes are ultrasonically dispersed in a tetrakis (4-aminophenyl) porphyrin solution, and the ultrasonic wave is also continued for a certain period of time before centrifugation. After repeating this process twice, the carbon nanotubes were taken out and dried. Finally, the obtained material is treated at 600-900 degrees Celsius for two hours under nitrogen or vacuum atmosphere to obtain the product. The method has the advantages of simple process, low equipment requirement, low energy consumption, and simple and easy-to-control reaction process; the obtained material exhibits good oxygen reduction reaction activity in an alkaline environment.

Description

technical field [0001] The invention relates to a carbon nanotube material wrapped with a nitrogen-containing amorphous carbon layer and a synthesis method thereof, specifically a highly active oxygen reduction containing nitrogen, carbon and iron elements with a carbon nanotube core-amorphous carbon layer shell structure Preparation method of reaction catalyst. Background technique [0002] Carbon materials are widely used in people's life because of their simple preparation, excellent performance and low cost. In recent years, the application range of carbon materials has been further expanded by loading metals or metal oxides on carbon supports or doping non-metallic heteroatoms in the lattice of carbon materials. Among the many modification methods for carbon materials, nitrogen doping has attracted much attention. Nitrogen atoms with strong electron-withdrawing ability can effectively reduce the electron cloud density on nearby carbon atoms, and then turn them into ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B82Y30/00B82Y40/00H01M4/90
CPCY02E60/50
Inventor 杨启华姚毅
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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