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Method for preparing mono-dispersed N-doped ordered mesoporous carbon spheres with particle size of 100-800 nm at high yield in single-pass mode

A monodisperse, nitrogen-doped technology, applied in the preparation/purification of carbon, nanotechnology for materials and surface science, nanotechnology, etc., can solve problems such as unfavorable large-scale production, complex synthesis steps, low single yield, etc. problems, to achieve the effect of saving solvent consumption, simple and easy preparation method, and good monodispersity

Active Publication Date: 2016-05-11
SHAANXI NORMAL UNIV +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the shortcomings of the existing nitrogen-doped ordered mesoporous carbon nanosphere preparation method, such as low single yield, unfavorable for large-scale production, uncontrollable shape, complicated synthesis steps, etc., to provide a A method for preparing nitrogen-doped ordered mesoporous carbon spheres with a particle size of 100-800 nm, which is simple, low in synthesis cost, short in synthesis time, and high in a single yield

Method used

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  • Method for preparing mono-dispersed N-doped ordered mesoporous carbon spheres with particle size of 100-800 nm at high yield in single-pass mode
  • Method for preparing mono-dispersed N-doped ordered mesoporous carbon spheres with particle size of 100-800 nm at high yield in single-pass mode
  • Method for preparing mono-dispersed N-doped ordered mesoporous carbon spheres with particle size of 100-800 nm at high yield in single-pass mode

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add F127 in the mixed solution of 416mL water and 104mL dehydrated alcohol, stir until F127 dissolves completely, the concentration of F127 in the gained solution is 4.6mmol / L; Add 16.70g (150mmol) 3-aminophenol, 10.62 g (75mmol) hexamethylenetetramine and 7.43mL (192.40mmol) ammonia water (mass fraction is 27%), the control stirring speed is 1080 rev / min, after stirring at room temperature for 60 minutes, 72 ℃ of stirring reaction 24 hours, the reaction The product was separated by centrifugation, washed three times with deionized water and absolute ethanol successively, and the obtained solid was dried at 60°C for 10 hours, and then dried under N 2 Under the atmosphere, the temperature was raised to 350°C, kept for 1 hour, and then the temperature was raised to 600°C for carbonization for 3 hours, and ground to obtain 6.5g of monodisperse nitrogen-doped ordered mesoporous carbon spheres with a particle size distribution of 100-400nm.

[0028] The obtained product adop...

Embodiment 2

[0037] Add F127 to the mixed solution of 416mL water and 104mL absolute ethanol, stir until F127 dissolves completely, the concentration of F127 in the gained solution is 4.6mmol / L; Then add 22.27g (200mmol) 3-aminophenol, 14.16 g (100mmol) hexamethylenetetramine and 7.43mL (192.40mmol) ammonia water (mass fraction is 27%), the control stirring speed is 1080 rpm, after stirring at room temperature for 60 minutes, 72 ℃ stirring reaction for 24 hours, the reaction The product was separated by centrifugation, washed three times with deionized water and absolute ethanol successively, and the obtained solid was dried at 60°C for 10 hours, and then dried under N 2 Under the atmosphere, the temperature was raised to 350°C, kept for 1 hour, then heated to 600°C for carbonization for 3 hours, and ground to obtain 10.5g of monodisperse nitrogen-doped ordered mesoporous carbon spheres with a particle size distribution of 100-800nm ​​(see Figure 8 ).

Embodiment 3

[0039] Add F127 to the mixed solution of 416mL water and 104mL absolute ethanol, stir until F127 dissolves completely, the concentration of F127 in the gained solution is 4.6mmol / L; Then add 33.41g (300mmol) 3-aminophenol, 21.24 g (150mmol) hexamethylenetetramine and 7.43mL (192.40mmol) ammonia water (mass fraction is 27%), the control stirring speed is 1080 rev / min, after stirring at room temperature for 60 minutes, 72 ℃ stirring reaction for 24 hours, the reaction The product was separated by centrifugation, washed three times with deionized water and absolute ethanol successively, and the obtained solid was dried at 60°C for 10 hours, and then dried under N 2 Under the atmosphere, the temperature was raised to 350°C, kept for 1 hour, then heated to 600°C for carbonization for 3 hours, and ground to obtain 20.0g of monodisperse nitrogen-doped ordered mesoporous carbon spheres with a particle size distribution of 100-800nm ​​(see Figure 9 ).

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Abstract

The invention discloses a method for preparing mono-dispersed N-doped ordered mesoporous carbon spheres with the particle size of 100-800 nm at high yield in a single-pass mode. According to the method, F127, 3-aminophenol and NH3.H2O serve as a template, a carbon and nitrogen source and a catalyst respectively, and the mono-dispersed N-doped ordered mesoporous carbon spheres with the particle size of 100-800 nm are produced at high yield in the single-pass mode on a large scale by regulating and controlling product morphology through ethyl alcohol. The preparing method is easy to implement, the concentration of the carbon and nitrogen source in the system is high, dosage of solvent is greatly reduced, several grams of N-doped ordered mesoporous carbon spheres can be obtained at high yield in the single-pass mode, the obtained N-doped ordered mesoporous carbon spheres are small in size distribution range, good in monodispersity and regular in pore structure and can be directly used as a catalyst, adsorbent and the like.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a method for preparing monodisperse nitrogen-doped ordered mesoporous carbon spheres with a particle size of 100-800 nm in a single high-yield process. Background technique [0002] Nitrogen-doped ordered mesoporous carbon materials have high application value in catalysis and other fields due to their unique pore structure, uniform pore channel, adjustable pore size, and easy surface modification. Catalyst etc. At present, the methods for preparing nitrogen-doped ordered mesoporous carbon materials mainly include post-processing method and direct synthesis method, and direct synthesis method includes hard template method and soft template method. The hard template method is to introduce nitrogen-carbon precursors into templates of porous materials with fixed mesostructures (such as SiO 2 Among the mesoporous molecular sieves), the product obtained ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02B82Y30/00B82Y40/00C01B32/05
CPCC01P2002/72C01P2004/03C01P2004/04C01P2004/32C01P2004/62C01P2004/64C01P2004/80C01P2006/12C01P2006/14C01P2006/16C01P2006/17
Inventor 陈沛杨佩赵凤起高红旭陈新兵安忠维
Owner SHAANXI NORMAL UNIV
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