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Nitrogen and boron co-doped carbon nano microspheres and preparation method thereof

A technology of carbon nano-microspheres and co-doping, which is applied in the direction of nano-carbon, etc., to achieve the effect of expanding the application field, regular shape and simple operation

Active Publication Date: 2017-08-22
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, through organic synthesis design, boron and nitrogen elements are introduced into monomers, polymerized to form polymer precursors and then carbonized to obtain boron and nitrogen doped carbon materials, and there are few reports

Method used

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  • Nitrogen and boron co-doped carbon nano microspheres and preparation method thereof
  • Nitrogen and boron co-doped carbon nano microspheres and preparation method thereof
  • Nitrogen and boron co-doped carbon nano microspheres and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0033] 1) Preparation of borate polymer microspheres:

[0034] 1-1) Dissolve tris(4-aminophenyl)amine (0.145g, 0.5mmol) and 3,4-dihydroxybenzaldehyde (0.207g, 1.5mmol) in 20mL ethanol, at room temperature (eg 25°C) The reaction was stirred at 400 rpm for 24 h in the dark. For kinetic research, samples are taken at set time intervals for GPC and NMR testing. After the reaction is completed, the black solution obtained is the catechol group-containing monomer TC.

[0035] The synthetic reaction formula of this catechol group monomer TC is as follows figure 1 as shown in a. The proton nuclear magnetic resonance spectrum ( 1 H NMR) and carbon nuclear magnetic resonance ( 13 C NMR) results such as figure 2 a and figure 2 As shown in c, the solvent is deuterated dimethyl sulfoxide (DMSO-D 6 ). The peak positions in the hydrogen spectrum are assigned as follows: 9.70(s,3H), 9.55(s,3H), 8.61(s,3H), 7.39(d,3H), 7.21(d,6H), 7.16(d,3H), 7.05 (d, 6H), 6.83 (d, 3H). The peak p...

Embodiment 2

[0046] 1) Preparation of borate polymer microspheres:

[0047] 1-1) Dissolve 5,10,15,20-tetrakis(4-aminophenyl)porphyrin (0.3374g, 0.5mmol) and 3,4-dihydroxybenzaldehyde (0.276g, 2mmol) in 20mL of ethanol , the reaction was stirred at 400 rpm for 24 h at room temperature (eg 25° C.) in the dark. For kinetic research, samples are taken at set time intervals for GPC and NMR testing. After the reaction is completed, the black solution obtained is the monomer PC containing catechol groups. The synthetic reaction formula of this catechol group monomer PC is as follows figure 1 as shown in c.

[0048] 1-2) Dissolve 5,10,15,20-tetrakis(4-aminophenyl)porphyrin (0.3374g, 0.5mmol) and 4-formylphenylboronic acid (0.3g, 2 mmol) in 20mL of ethanol, The reaction was stirred at 400 rpm for 24 h at room temperature (eg, 25° C.) in the dark. For kinetic research, samples are taken at set time intervals for GPC and NMR testing. After the reaction is completed, the dark yellow solution obt...

Embodiment 3～4

[0054] Embodiments 3 to 4: With reference to the process conditions of Example 1, in the step of preparing borate polymer microspheres, the ratio between the monomer containing catechol group and the monomer containing phenylboronic acid group was changed, and the synthesis was different. The morphology of borate polymer microspheres was used to prepare nitrogen and boron co-doped carbon nanospheres, as shown in Table 1.

[0055] Table 1 Reaction conditions for the synthesis of borate polymer microspheres with different morphologies in Examples 3-4

[0056]

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Abstract

The invention relates to nitrogen and boron co-doped carbon nano microspheres and a preparation method thereof. The preparation method comprises the following steps of: firstly, performing reactions on a polyamino compound with 3,4-dihydroxyl benzaldehyde and 4-formylphenylboronic acid to synthesize a monomer with a pyrocatechol group and a phenylboronic acid group; then performing a condensation reaction on pyrocatechol and boric acid to prepare borate polymer microspheres containing nitrogen and boron; carbonizing the microspheres by way of high-temperature calcining; and finally, forming the nitrogen and boron co-doped carbon nano microspheres. The method can synergically dope nitrogen and boron in the carbon nano microspheres and has a potential advantage in enhancing the capacitance and electro-catalytic property and the like of the carbon nano material.

Description

technical field [0001] The invention belongs to the field of hybrid nanomaterials, and in particular relates to a nitrogen and boron co-doped carbon nanometer sphere and a preparation method thereof. Background technique [0002] Due to their excellent physical and chemical properties, carbon materials such as carbon nanowires, carbon nanotubes, graphite, and graphene have shown outstanding application value in the fields of modern energy, catalysis, and life medicine. It is worth mentioning that in the field of energy and catalysis, heteroelement doping has attracted extensive attention because it can significantly improve the catalytic performance and stability of carbon materials. Among them, nitrogen-doped carbon catalyst is the earliest, most widely studied and currently the best heteroelement-doped carbon catalyst. Compared with nitrogen single doping, multi-element co-doping has significant advantages in improving the electrochemical performance of carbon materials. ...

Claims

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Application Information

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IPC IPC(8): C01B32/15
CPCC01P2004/03C01P2004/04C01P2004/32C01P2004/52C01P2004/62C01P2004/80
Inventor 袁丛辉武彤戴李宗毛杰许一婷曾碧榕罗伟昂陈国荣
Owner XIAMEN UNIV
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