Preparation method for pressure-assisted size-controllable hydrothermal carbon spheres and prepared hydrothermal carbon spheres

A hydrothermal carbon and size technology, applied in the preparation/purification of carbon, nano-carbon, etc., can solve the problems of poor size controllability and narrow adjustable size of carbon balls, and achieve uniform size, good size uniformity, and improved stability. sexual effect

Active Publication Date: 2018-12-11
SHAANXI UNIV OF SCI & TECH
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Problems solved by technology

[0004] Aiming at the problems existing in the prior art, the present invention provides a method for preparing pressure-assisted size-controllable hydrothermal carbon spheres and the prepared hydrothermal carbon spheres, so as to solve the problem of narrow adjustable size and controllable size of carbon spheres in the prior art. sex problem

Method used

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  • Preparation method for pressure-assisted size-controllable hydrothermal carbon spheres and prepared hydrothermal carbon spheres
  • Preparation method for pressure-assisted size-controllable hydrothermal carbon spheres and prepared hydrothermal carbon spheres
  • Preparation method for pressure-assisted size-controllable hydrothermal carbon spheres and prepared hydrothermal carbon spheres

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preparation example Construction

[0028] The preparation method of pressure-assisted size-controllable hydrothermal carbon spheres of the present invention comprises the following steps:

[0029] S1. Configure the concentration of glucose solution to be 0.1M-2M;

[0030] S2. Put the glucose solution obtained in step S1 into the autoclave, seal the autoclave, and feed gas through the air inlet on the autoclave to increase the pressure by 0.5-3.0 MPa, that is, pressurize to 0.6-3.1 MPa;

[0031] S3. Heating the autoclave in step S2 to 160-220° C. for 2-12 hours, then cooling to room temperature;

[0032] S4. Washing and drying the product obtained in step S3 to obtain the target product.

[0033] In the step S2, the glucose solution is placed in an autoclave and sealed with a thread.

[0034] The dosage of the glucose solution is 1 / 3-2 / 3 of the volume of the autoclave.

[0035] Said pressurization is to remove the self-generated pressure produced by the autoclave at room temperature, and the extra increased p...

Embodiment 1

[0041] 1) Configure the concentration of glucose solution as 1M;

[0042] 2) Take 60mL of the glucose solution with the above concentration, put it into a 100mL autoclave, seal it, feed nitrogen gas to increase the pressure by 0.5MPa, heat to 200°C for 12h, and naturally cool to room temperature after the reaction to obtain a carbon sphere solution.

[0043] 3) Centrifuge the above solution at 3000r / min, and repeatedly ultrasonically disperse and centrifuge with absolute ethanol and deionized water until the cleaning solution is clear.

[0044] 4) Dry the above-mentioned cleaned carbon spheres in a vacuum oven at 60° C. for 12 hours to obtain hydrothermal carbon spheres.

[0045] figure 1 Shown is the scanning electron microscope image of the carbon spheres obtained in Example 1. It can be seen from the figure that the carbon spheres have uniform size and good dispersion, and the size is about 200nm.

Embodiment 2

[0047] 1) Configure the concentration of glucose solution to be 0.5M;

[0048] 2) Take 60mL of the glucose solution with the above concentration, put it into a 100mL autoclave, seal it, feed nitrogen gas to increase the pressure by 1.0MPa, heat to 180°C for 10h, and naturally cool to room temperature after the reaction to obtain a carbon sphere solution.

[0049] 3) Centrifuge the above solution at 5000r / min, and repeatedly ultrasonically disperse and centrifuge with absolute ethanol and deionized water until the cleaning solution is clear.

[0050] 4) Dry the above-mentioned cleaned carbon spheres in a vacuum oven at 60° C. for 12 hours to obtain hydrothermal carbon spheres.

[0051] figure 2 Shown is the scanning electron microscope image of the carbon spheres obtained in Example 2. It can be seen from the figure that the carbon spheres have a uniform diameter, good dispersion, and a size of about 800 nm.

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Abstract

The invention provides a preparation method for pressure-assisted size-controllable hydrothermal carbon spheres and the prepared hydrothermal carbon spheres. The method comprises the following steps of S1, preparing a glucose solution; S2, putting the glucose solution prepared in the step S1 into a high-pressure kettle, sealing the high-pressure kettle, and introducing gas into the high-pressure kettle through a gas inlet on the high-pressure kettle for pressurization to reach 0.6-3.1 MPa; S3, heating the high-pressure kettle in the step S2 for hydrothermal reaction; and S4, washing and dryinga product obtained in the step S3 so as to obtain the hydrothermal carbon spheres. According to the preparation method and the prepared hydrothermal carbon spheres, by changing the pressure, the hydrothermal carbon spheres with adjustable size within the range of 60 nanometers-2 microns, good dispersity and uniform size can be efficiently prepared, and therefore, the stability of the performanceof the carbon spheres can be improved.

Description

technical field [0001] The invention belongs to the field of preparation of micro-nano carbon spheres, in particular to a method for preparing pressure-assisted size-controllable hydrothermal carbon spheres and the prepared hydrothermal carbon spheres. Background technique [0002] Hydrothermal carbon spheres are widely used in catalyst supports, supercapacitors, drug loading, templates and adsorption due to their mild preparation conditions and abundant surface oxygen-containing functional groups. Compared with traditional chemical vapor deposition, high-temperature carbonization, and arc discharge methods to prepare carbon spheres, hydrothermal carbon spheres are more environmentally friendly, and the raw materials used, such as glucose, are also renewable and sustainable. Controllable size and size uniformity are very important for the stability of carbon spheres performance, however, carbon spheres prepared by traditional hydrothermal method often have poor size controll...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15C01B32/05
CPCC01B32/05C01B32/15
Inventor 张素风张璐璐钱立伟杨金帆敖志锋张宏宇
Owner SHAANXI UNIV OF SCI & TECH
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