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Preparation method of nitrogen-doped carbon material with high nitrogen content

A technology of nitrogen-doped carbon and high nitrogen content, applied in the direction of nano-carbon, etc., to achieve the effects of wide applicability, simple process, and adjustable nitrogen doping types

Active Publication Date: 2020-10-13
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the nitrogen content of nitrogen-doped carbon materials prepared by conventional direct carbonization of traditional polymer organics is often limited by the carbonization temperature, and the nitrogen content in the resulting carbonized products is often much lower than that of its polymer precursors. Nitrogen content in

Method used

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  • Preparation method of nitrogen-doped carbon material with high nitrogen content
  • Preparation method of nitrogen-doped carbon material with high nitrogen content
  • Preparation method of nitrogen-doped carbon material with high nitrogen content

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 91.6 milliliters of aniline was dissolved in 800 milliliters of aqueous hydrochloric acid (1.25 moles per liter) to obtain solution A, and 228.8 grams of ammonium thiosulfate was dissolved in 400 milliliters of deionized water to obtain solution B. Cool solutions A and B to 4°C, then add solution B to solution A at one time under stirring (1000 rpm), and continue stirring for 24 hours. The resulting solid was filtered, washed with deionized water, and dried (overnight in an oven at 120 degrees Celsius) to obtain polyaniline. The above freshly prepared dried polyaniline was placed in a muffle furnace, and oxidized and pretreated at 120, 250, 300, 350, 400 and 450 degrees Celsius for 3 hours under an air atmosphere to obtain a partially cross-linked polyaniline precursor body. Then the above precursor was transferred to a tube furnace, and carbonized at 800 °C (heating rate 2 °C per minute) for 6 hours under a nitrogen atmosphere to prepare a nitrogen-doped carbon materi...

Embodiment 2

[0027] The dried polyaniline freshly prepared in Example 1 was placed in a muffle furnace, and oxidized and pretreated at 350 degrees under an air atmosphere for 0.5 hours, 1 hour, 10 hours, 24 hours and 48 hours respectively to obtain partial crossover. linked polyaniline precursors. Then the above precursor was transferred to a tube furnace, and carbonized at 800 °C (heating rate 2 °C per minute) for 6 hours under a nitrogen atmosphere to prepare a nitrogen-doped carbon material. Combined with the results of Examples 1 and 2, it is shown that the nitrogen-doped carbon material obtained by carbonizing polyaniline after oxidation pretreatment at 350 degrees Celsius in the air for 1-3 hours has a significant increase in nitrogen content; The increase in content was not obvious.

Embodiment 3

[0029] The dried polyaniline freshly prepared in Example 1 was placed in a muffle furnace, and oxidized and pretreated at 350° C. for 3 hours under an air atmosphere to obtain a partially crosslinked polyaniline precursor. Then the above precursors were transferred to a tube furnace, and carbonized at 800 °C (heating rates of 0.5, 1, and 5 °C per minute) under a nitrogen atmosphere for 6 hours to prepare nitrogen-doped carbon materials. Combining the results of Examples 1 and 3, it is shown that the heating rate is best at 0.5-2 degrees Celsius per minute, and the nitrogen content of the nitrogen-doped carbon material obtained by continuing to increase the heating rate decreases.

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Abstract

The invention discloses a preparation method of a nitrogen-doped carbon material with high nitrogen content. The preparation method comprises the following steps: (1) putting a dried nitrogen-containing polymer organic matter into a muffle furnace or a tubular furnace, and carrying out oxidation pretreatment for a certain time at a certain temperature in an oxygen-containing atmosphere to obtain apartially cross-linked nitrogen-containing polymer organic matter precursor; and (2) transferring the partially cross-linked nitrogen-containing polymer organic matter precursor into a tubular furnace, and carbonizing at a certain temperature in an inert atmosphere to obtain the nitrogen-doped carbon material. The method disclosed by the invention has the following remarkable advantages: (1) thetechnological process is relatively simple; (2) the content of nitrogen in the obtained nitrogen-doped carbon material is high; (3) the nitrogen doping type is adjustable; and (4) the method has wideapplicability to various nitrogen-containing polymer organic matters.

Description

technical field [0001] The invention relates to the technical field of carbon material preparation, in particular to a preparation method of nitrogen-doped carbon material with high nitrogen content. Background technique [0002] Carbon nanomaterials usually have excellent acid and alkali resistance, good mechanical properties and electrical conductivity, high specific surface area, and rich surface physical and chemical properties, so they have a wide range of applications in the fields of gas adsorption and separation, electrochemistry, and energy storage materials. Value. It is an important means to synthesize new functional carbon materials by introducing second components, such as nitrogen, boron, sulfur, and phosphorus, into the carbon matrix. Among them, nitrogen doping has received extensive attention. Since the atomic radii of carbon and nitrogen are similar, it is easier for nitrogen to enter the skeleton of the carbon matrix. This doped carbon material not only...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15
CPCC01B32/15
Inventor 林荣和丁云杰
Owner ZHEJIANG NORMAL UNIVERSITY