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A kind of preparation method of nitrogen-doped ultramicroporous carbon nanosphere

A carbon nanosphere, nitrogen doping technology, applied in nanocarbon, nanotechnology, nanotechnology and other directions, can solve the problems of large particle size of carbon nanospheres, complex preparation methods, low specific surface area, etc., to reduce shrinkage and collapse, Simple preparation process

Inactive Publication Date: 2018-02-09
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The carbon nanospheres prepared by these methods have the disadvantages of large particle size (more than 100nm), or low specific surface area, or complicated preparation methods.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Phloroglucinol, terephthalaldehyde, water, resorcinol, hexamethylenetetraammonium and formaldehyde are taken in an amount of 1:0.79:445:2.62:0.49:1.29 in parts by mass. First react phloroglucinol, terephthalaldehyde and water at 70° C. for 1 hour at a stirring speed of 450 rpm to obtain a solution containing phloroglucinol / terephthalaldehyde polymer nanoparticles. Add resorcinol and hexamethylenetetramine to the solution containing phloroglucinol / terephthalaldehyde polymer nanoparticles, then add formaldehyde dropwise to the above solution at a stirring speed of 450 rpm React at 35°C for 24h to obtain a nitrogen-doped polymer solution. The solution was subjected to hydrothermal treatment at 100° C. for 24 hours, and the obtained product was dried at 70° C. for 48 hours to obtain polymer nanospheres. In a tube furnace, the temperature was raised from room temperature to 700°C for carbonization at a rate of 2°C / min under a nitrogen atmosphere and kept for 6 hours, and th...

Embodiment 2

[0016] Phloroglucinol, terephthalaldehyde, water, resorcinol, hexamethylenetetramine and formaldehyde are taken in the quantity of 1:0.79:445:2.62:0.74:1.29 parts by mass. First react phloroglucinol, terephthalaldehyde and water at 70° C. for 1 hour at a stirring speed of 500 rpm to obtain a solution containing phloroglucinol / terephthalaldehyde polymer nanoparticles. Add resorcinol and hexamethylenetetramine to the solution containing phloroglucinol / terephthalaldehyde polymer nanoparticles, then add formaldehyde dropwise to the above solution, at a stirring speed of 500 rpm React at 35°C for 24h to obtain a nitrogen-doped polymer solution. The solution was subjected to hydrothermal treatment at 100° C. for 24 hours, and the obtained product was dried at 70° C. for 48 hours to obtain polymer nanospheres. In a tube furnace, the temperature was raised from room temperature to 850°C for carbonization at a rate of 5°C / min under a nitrogen atmosphere and kept for 4 hours, and the n...

Embodiment 3

[0018] Phloroglucinol, terephthalaldehyde, water, resorcinol, hexamethylenetetramine and formaldehyde are taken in parts by mass of 1:0.79:445:2.62:2:3. First react phloroglucinol, terephthalaldehyde and water at 70° C. for 1 hour at a stirring speed of 700 rpm to obtain a solution containing phloroglucinol / terephthalaldehyde polymer nanoparticles. Add resorcinol and hexamethylenetetramine to the solution containing phloroglucinol / terephthalaldehyde polymer nanoparticles, then add formaldehyde dropwise to the above solution, at a stirring speed of 700 rpm React at 35°C for 24h to obtain a nitrogen-doped polymer solution. The solution was subjected to hydrothermal treatment at 110° C. for 24 hours, and the obtained product was dried at 120° C. for 24 hours to obtain polymer nanospheres. In a tube furnace, the temperature was raised from room temperature to 850°C for carbonization at a rate of 8°C / min under a nitrogen atmosphere and kept for 4 hours, and the temperature was nat...

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Abstract

The invention relates to a preparation method of nitrogen-doped ultramicroporous carbon nanospheres, belonging to the technical field of material preparation. The preparation method comprises the following steps: weighing 1 part by mass of phloroglucin, 0.79 part by mass of terephthalaldehyde, 445 parts by mass of water, 2.62 parts by mass of resorcinol, 0.49-4.45 parts by mass of hexamethylene tetraammonia and 1.29-3.86 parts by mass of formaldehyde; mixing the phloroglucin, terephthalaldehyde water, stirring, reacting at 70 DEG C for 1 hour, adding the resorcinol, hexamethylene tetraammonia and formaldehyde, and reacting at 35 DEG C for 24 hours, thereby obtaining a nitrogen-doped polymer solution; carrying out hydrothermal treatment on the solution at 100-110 DEG C for 24 hours, and drying the obtained product to obtain polymer nanospheres; and in a tube furnace, heating from room temperature to 700-900 DEG C at the heating rate of 2-10 DEG C / minute in a nitrogen atmosphere to perform carbonization, keeping for 4-6 hours, and naturally cooling to obtain the nitrogen-doped ultramicroporous carbon nanospheres. The nitrogen-doped ultramicroporous carbon nanospheres have the advantages of simple technique, uniform particle size and large specific area, and have important application prospects in the fields of energy storage and conversion and the like.

Description

technical field [0001] The invention relates to a preparation method of nitrogen-doped ultramicroporous carbon nanospheres, belonging to the technical field of material preparation. Background technique [0002] Carbon nanospheres are a new type of carbon nanomaterial with a spherical structure. It has the advantages of regular shape and controllable particle size. It has a wide range of applications in energy storage, adsorption, catalysis and other fields. For example, "a single-layer and multi-layer hollow carbon nanosphere, preparation and application" (Chinese invention patent, application number: 201510137088.6), "a preparation method of mesoporous imprinted carbon nanosphere" (Chinese invention patent, application No.: 201410499699.0), "Carbon Nanospheres and Its Preparation Method and Application" (Chinese Invention Patent, Application No.: 201210504772.X), etc. These reports disclose the preparation methods of carbon nanospheres and their applications in adsorption...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/15B82Y30/00
CPCB82Y30/00C01P2004/32C01P2004/64C01P2006/12C01P2006/16
Inventor 刘明贤陆文静甘礼华
Owner TONGJI UNIV