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Preparation method of size-controllable microporous carbon nanorod

A technology of nanorods and microporous carbon, which is applied in the field of preparation of microporous carbon nanorods, which can solve the problems of uncontrollable size of microporous carbon materials, large size of MOF template materials, and long synthesis time, so as to achieve uniform appearance and low cost. Effect of low cost and high specific surface area

Inactive Publication Date: 2017-06-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, although there are many researches on the preparation of carbon materials using MOF template materials, there are still the following deficiencies: 1. Most MOF template materials use solvothermal and direct heating synthesis methods, and the synthesis takes a long time (Nanoscale, 2014, 6, 4387–4394); 2. The size of the MOF template material is large and the shape is uneven (Bulletin of the Korean Chemical Society, 2009, 30, 2921-2926); 3. The size of the microporous carbon material cannot be in the small size range effective regulation within

Method used

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  • Preparation method of size-controllable microporous carbon nanorod
  • Preparation method of size-controllable microporous carbon nanorod

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Mix the ethanol solution of trimesic acid and the aqueous solution of zinc acetate dihydrate, and conduct an ultrasonic reaction at 25° C. for 30 minutes under the conditions of ultrasonic frequency 53 KHz and power 500 W. The molar concentration of trimesic acid is 0.0125mol / L, the molar ratio of trimesic acid to zinc acetate dihydrate is 1:1, and the volume content of water is 12.5%. Centrifuge, wash, and dry to obtain the zinc metal organic framework material; calcinate at 800° C. for 5 h under a nitrogen atmosphere, soak in 10% hydrofluoric acid for 12 h to remove metal oxides, and obtain microporous carbon nanorods.

Embodiment 2

[0028] Mix the ethanol solution of trimesic acid and the aqueous solution of zinc acetate dihydrate, and conduct an ultrasonic reaction at 25° C. for 30 minutes under the conditions of ultrasonic frequency 53 KHz and power 500 W. The molar concentration of trimesic acid is 0.0125mol / L, the molar ratio of trimesic acid to zinc acetate dihydrate is 1:1, and the volume content of water is 25%. Centrifuge, wash, and dry to obtain the zinc metal organic framework material; calcinate at 800° C. for 5 h under a nitrogen atmosphere, soak in 10% hydrofluoric acid for 12 h to remove metal oxides, and obtain microporous carbon nanorods.

Embodiment 3

[0030] Mix the ethanol solution of trimesic acid and the aqueous solution of zinc acetate dihydrate, and conduct an ultrasonic reaction at 25°C for 30 minutes under the conditions of ultrasonic frequency 53KHz and power 500W. The molar concentration of trimesic acid is 0.0125mol / L, the molar ratio of trimesic acid to zinc acetate dihydrate is 1:1, and the volume content of water is 50%. Centrifuge, wash, and dry to obtain the zinc metal organic framework material; calcinate at 800° C. for 5 h under a nitrogen atmosphere, soak in 10% hydrofluoric acid for 12 h to remove metal oxides, and obtain microporous carbon nanorods.

[0031] The difference between embodiment 4-8 and embodiment 1 is shown in the table below:

[0032]

[0033]

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Abstract

The invention relates to a preparation method of a size-controllable microporous carbon nanorod. The preparation method comprises the following steps: quickly synthesizing rod-shaped metal organic skeleton materials with different sizes by a low-concentration ultrasonic method and by adjusting the water volume content (12.5 to 50 percent) of a reaction system; performing high-temperature carbonization to obtain a metal oxide / carbon composite material by taking a metal organic skeleton material as a template and a carbon source; dissolving by using an acid liquid to remove metal oxide to prepare the microporous carbon nanorod with an extremely high specific surface and a developed pore structure. The lower the water content of the reaction system is, the less the size of the microporous carbon nanorod is and the narrower the size distribution is. The microporous carbon nanorod provided by the invention is uniform in appearance, adjustable in size, simple in preparation process, high in yield, low in cost and suitable for batch production.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of inorganic non-metallic nanometer materials, in particular to a preparation method of microporous carbon nanorods with controllable size. Background technique [0002] Due to the characteristics of high mechanical and thermal stability, good electrical conductivity, and high specific surface area, microporous carbon materials have shown great potential in the fields of energy storage, fuel cells, supercapacitors, catalysis and gas separation, and medicine. Excellent application value has become a research hotspot in recent years. [0003] Metal-organic framework (MOF) materials are self-assembled from metal ion coordination centers and binary, ternary or quaternary organic oxygen-containing carboxylic acid ligands in solvents. Using MOF as a template to prepare microporous carbon materials has become a hotspot of recent research. Using MOF as a template, by introducing carbon sourc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15B82Y40/00
Inventor 吴仁安徐桂菊牛欢
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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