Preparation method of nitrogen-doped porous-structure carbon material

Abstract

The invention discloses a preparation method of a nitrogen-doped porous-structure carbon material and belongs to the technical field of inorganic material preparation. The preparation method utilizes a micromolecular carbon-containing compound as a raw material and comprises the following steps of based on the weight of the raw material, adding 0-400wt% of an inorganic base, 0-400wt% of an organic nitrogen-containing compound and 0-50wt% of a metal or metal oxide or inorganic metal salt into the raw material, carrying out uniform dispersion, and carrying out a reaction process in an inert gas protective atmosphere at a temperature of 400-900 DEG C for 0.5-12h so that the nitrogen-doped porous-structure carbon material having micropores, mesopores and macropores is obtained. The preparation method has simple processes, can be controlled easily, and realizes one-step combination of porous structure, functionalization nitrogen doping and metal particle modification. The nitrogen-doped porous-structure carbon material having high nitrogen content has a large capacitance value and good cycle performances, can be used as an oxygen reduction reaction catalyst having high activity, high selectivity and high stability and has a very large application prospect.

Description

technical field

[0001] The invention relates to a method for preparing a nitrogen-doped porous structure carbon material, which belongs to the technical field of inorganic material preparation technology. technical background

[0002] Nitrogen-doped porous carbon materials have a wide range of industrial applications, including applications in supercapacitors, oxygen reduction catalysts, catalyst supports, adsorbents, energy storage materials, carbon dioxide capture and storage, and other fields. The use of it in supercapacitors, oxygen reduction catalysts, carbon dioxide capture and storage, etc. are all frontier topics in modern scientific and technological research. (See literature: Angew.Chem.Int.Ed.2008,47,373-376; ACS NANO 2012,6,7092-7102; Chem.Mater.2010,22,2178–2180; Angew.Chem.Int.Ed.2012, 51, 7480-7484; Chem.Mater.2012, 24, 464-470; Environ.Sci.Technol.2012, 46, 7407-7414;)

[0003] However, the existing nitrogen-doped porous carbon materials are usually prepare...

Examples

Embodiment 1

[0030] Example 1: Preparation of Nitrogen-doped Porous Structure Carbon Materials Using Small Molecule Carbon-Containing Compounds as Raw Materials

[0031] Take 4 grams of ethylenediaminetetraacetic acid, grind them evenly with 2 grams of potassium hydroxide, transfer them to a heating container, and react at 600°C for 2 hours under the protection of nitrogen. The obtained product is washed three times with deionized water, three times with ethanol, and dried A nitrogen-doped porous carbon material can be obtained. The obtained material has a porous structure, high specific capacitance value and good cycle performance. SEM photo see figure 1 , the capacitive cyclic voltammogram see figure 2 , the capacitance characteristic diagram see image 3 , the capacitance cycle diagram see Figure 4 , X-ray photoelectron spectroscopy see Figure 5 .

[0032] Repeat the above steps, and use 4 grams of ethylenediaminetetraacetic acid instead, 0.5 grams of potassium hydroxide, at a ...

Embodiment 2

[0040] Example 2: Preparation of nitrogen-doped porous structure carbon material from a mixture of small molecule carbon-containing compounds

[0041] Take 2 grams of ethylenediaminetetraacetic acid and 2 grams of dipotassium ethylenediaminetetraacetic acid, grind them evenly with 2 grams of potassium hydroxide, transfer them to a heating container, and react at 600 ° C for 2 hours under the protection of nitrogen, and the obtained product is washed with deionized water Washing three times, washing three times with ethanol, and drying can obtain nitrogen-doped porous structure carbon material. (SEM image see Image 6 )

[0042] Repeat the above operation steps, keep 2 grams of EDTA, 2 grams of potassium hydroxide, add 2 grams of disodium EDTA, and calcining for 1 hour at a temperature of 700 ° C under nitrogen protection to obtain similar products.

[0043] Repeat the above operation steps, keep 2 grams of EDTA, 0.5 grams of potassium hydroxide, add 2 grams of dipotassium ED...

Embodiment 3

[0052] Example 3: Adding organic nitrogen-containing compounds to prepare porous structure carbon materials with high nitrogen content

[0053] Take 4 grams of ethylenediamine tetraacetic acid and 2 grams of potassium hydroxide, grind them evenly with 2 grams of melamine, transfer them to a heating container, and react at 700°C for 2 hours under the protection of nitrogen. The obtained product is washed three times with deionized water and three times with ethanol , drying nitrogen-doped porous carbon material can be obtained (the scanning electron microscope picture is shown in Figure 7 , TEM pictures see Figure 8 )

[0054] Repeat the above operation steps, keep EDTA consumption 4 grams, potassium hydroxide 2 grams, add 16 grams of hexamethylenetetramine, temperature 600 ° C, calcining for 2 hours under nitrogen protection, similar products can be obtained.

[0055] Repeat the above operation steps, keep EDTA consumption 4 grams, potassium hydroxide 2 grams, add urea 2 g...

technical field

[0001] The invention relates to a method for preparing a nitrogen-doped porous structure carbon material, which belongs to the technical field of inorganic material preparation technology. technical background

[0002] Nitrogen-doped porous carbon materials have a wide range of industrial applications, including applications in supercapacitors, oxygen reduction catalysts, catalyst supports, adsorbents, energy storage materials, carbon dioxide capture and storage, and other fields. The use of it in supercapacitors, oxygen reduction catalysts, carbon dioxide capture and storage, etc. are all frontier topics in modern scientific and technological research. (See literature: Angew.Chem.Int.Ed.2008,47,373-376; ACS NANO 2012,6,7092-7102; Chem.Mater.2010,22,2178–2180; Angew.Chem.Int.Ed.2012, 51, 7480-7484; Chem.Mater.2012, 24, 464-470; Environ.Sci.Technol.2012, 46, 7407-7414;)

[0003] However, the existing nitrogen-doped porous carbon materials are usually prepare...

Examples

Embodiment 1

[0030] Example 1: Preparation of Nitrogen-doped Porous Structure Carbon Materials Using Small Molecule Carbon-Containing Compounds as Raw Materials

[0031] Take 4 grams of ethylenediaminetetraacetic acid, grind them evenly with 2 grams of potassium hydroxide, transfer them to a heating container, and react at 600°C for 2 hours under the protection of nitrogen. The obtained product is washed three times with deionized water, three times with ethanol, and dried A nitrogen-doped porous carbon material can be obtained. The obtained material has a porous structure, high specific capacitance value and good cycle performance. SEM photo see figure 1 , the capacitive cyclic voltammogram see figure 2 , the capacitance characteristic diagram see image 3 , the capacitance cycle diagram see Figure 4 , X-ray photoelectron spectroscopy see Figure 5 .

[0032] Repeat the above steps, and use 4 grams of ethylenediaminetetraacetic acid instead, 0.5 grams of potassium hydroxide, at a ...

Embodiment 2

[0040] Example 2: Preparation of nitrogen-doped porous structure carbon material from a mixture of small molecule carbon-containing compounds

[0041] Take 2 grams of ethylenediaminetetraacetic acid and 2 grams of dipotassium ethylenediaminetetraacetic acid, grind them evenly with 2 grams of potassium hydroxide, transfer them to a heating container, and react at 600 ° C for 2 hours under the protection of nitrogen, and the obtained product is washed with deionized water Washing three times, washing three times with ethanol, and drying can obtain nitrogen-doped porous structure carbon material. (SEM image see Image 6 )

[0042] Repeat the above operation steps, keep 2 grams of EDTA, 2 grams of potassium hydroxide, add 2 grams of disodium EDTA, and calcining for 1 hour at a temperature of 700 ° C under nitrogen protection to obtain similar products.

[0043] Repeat the above operation steps, keep 2 grams of EDTA, 0.5 grams of potassium hydroxide, add 2 grams of dipotassium ED...

Embodiment 3

[0052] Example 3: Adding organic nitrogen-containing compounds to prepare porous structure carbon materials with high nitrogen content

[0053] Take 4 grams of ethylenediamine tetraacetic acid and 2 grams of potassium hydroxide, grind them evenly with 2 grams of melamine, transfer them to a heating container, and react at 700°C for 2 hours under the protection of nitrogen. The obtained product is washed three times with deionized water and three times with ethanol , drying nitrogen-doped porous carbon material can be obtained (the scanning electron microscope picture is shown in Figure 7 , TEM pictures see Figure 8 )

[0054] Repeat the above operation steps, keep EDTA consumption 4 grams, potassium hydroxide 2 grams, add 16 grams of hexamethylenetetramine, temperature 600 ° C, calcining for 2 hours under nitrogen protection, similar products can be obtained.

[0055] Repeat the above operation steps, keep EDTA consumption 4 grams, potassium hydroxide 2 grams, add urea 2 g...

Images