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Kieselguhr template carbon with large specific surface area and high pore volume and preparation method thereof

A technology with large specific surface area and diatomite, applied in the preparation/purification of carbon, etc., can solve the problems of poor adsorption capacity, difficulty in popularization and application of diatomite-based porous carbon, low specific surface area and total pore volume, etc. Effect of Micropore Volume

Active Publication Date: 2013-03-13
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the diatomite template carbon prepared by the above method has the following problems: the pore structure is dominated by macropores, only a small amount of mesopores and micropores, and the specific surface area and total pore volume are low (much lower than commercial activated carbon: Usually specific surface>800m 2 / g, pore volume>0.50cm 3 / g), etc., resulting in poor adsorption capacity of the carbon material for gas and liquid small molecules, making it difficult to achieve direct industrial application.
Therefore, the diatomite-based porous carbon prepared by the above preparation method is difficult to popularize and apply.

Method used

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  • Kieselguhr template carbon with large specific surface area and high pore volume and preparation method thereof
  • Kieselguhr template carbon with large specific surface area and high pore volume and preparation method thereof
  • Kieselguhr template carbon with large specific surface area and high pore volume and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Weigh 1g of Jilin diatomite raw material purified by sedimentation (the main diatom species of which is diatoms of the order Diatomaceae) at room temperature and add it to 5ml of furfuryl alcohol, and then add 0.1g of oxalic acid to form a suspension. The resulting suspension was fully stirred for 1 hour; then placed in a vacuum drying oven, heated to 95° C. under vacuum, and a solid product was obtained after constant temperature for 2 hours.

[0026] 2) Put the above product in a tube furnace, raise the temperature to 700° C. under a nitrogen atmosphere, and keep the temperature constant for 3 hours to obtain a diatomite-carbon composite without removing the template. Then the nitrogen purging was stopped, and water vapor was introduced, and activated at a constant temperature of 700° C. for 1 hour, cooled to room temperature, and pulverized to obtain an activated solid.

[0027] 3) Add 1 g of the activated solid into 10 ml of 40% hydrofluoric acid solution by volu...

Embodiment 2

[0031] 1) Weigh 1g of Jilin diatomite raw material purified by sedimentation (the main diatom species of which is diatoms of the order Diatomaceae) at room temperature and add it to 5ml of furfuryl alcohol, and then add 0.1g of oxalic acid to form a suspension. The resulting suspension was fully stirred for 1 hour; then placed in a vacuum drying oven, heated to 95° C. under vacuum, and a solid product was obtained after constant temperature for 2 hours.

[0032] 2) Put the above product in a tube furnace, raise the temperature to 700° C. under a nitrogen atmosphere, and keep the temperature constant for 3 hours to obtain a diatomite-carbon composite without removing the template. Then the nitrogen purge was stopped, and CO 2 , and activated at a constant temperature of 700 ° C for 1 hour, cooled to room temperature, and pulverized to obtain an activated solid.

[0033] 3) Add 1 g of the activated solid into 10 ml of 40% hydrofluoric acid solution by volume, and stir thoroughl...

Embodiment 3

[0037] This embodiment is basically the same as Embodiment 2, except that it is activated for 2 hours under a carbon dioxide atmosphere, and other steps are the same.

[0038] Through high-resolution scanning electron microscope observation, it is found that the obtained diatomite template carbon replicates the densely arranged tubular morphology of diatomite. Through transmission electron microscope observation, it is found that it has a macroporous tubular structure, and there are abundant mesopores and micropores on the surface of the tube wall. The specific surface area of ​​the large specific surface area and high pore volume diatomite template carbon obtained in this example is 1275m 2 / g, the total pore volume is 0.797cm 3 / g, the micropore volume is 0.321cm 3 / g( figure 2 in c), the micropore pore sizes are concentrated at ~0.7 and 1 nm ( image 3 in c).

[0039] As an application, the ability of the large specific surface area and high pore volume diatomite temp...

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Abstract

The invention discloses a kieselguhr template carbon with large specific surface area and high pore volume, and a preparation method of the kieselguhr template carbon. The method comprises the following steps in sequence: carbonizing kieselguhr to obtain a kieselguhr-carbon complex with the template contained; transferring the kieselguhr-carbon complex with the template contained into the atmosphere of steam or carbon dioxide; heating to 700 to 900 DEG C; fully roasting for 1 to 3 hours; crushing to obtain the activated solid; removing the template from the activated solid; and washing and drying to obtain the kieselguhr template carbon with large specific surface area and high pore volume. The kieselguhr template carbon with large specific surface area and high pore volume, prepared by the preparation method disclosed by the invention, is outstanding in properties and methylene blue adsorption capacity, can be widely applied to the fields such as the adsorption field, the separation field, the load field and the capacitor preparation field, and is wide in the application prospect. The method has the advantages of being low in cost, simple in process, high in efficiency, less in pollution, and low in energy consumption.

Description

Technical field: [0001] The invention relates to a diatomite-based porous carbon and a preparation method thereof, in particular to a diatomite template carbon with a large specific surface area and a high pore volume and a preparation method thereof. Background technique: [0002] Porous carbon has the characteristics of rich pore structure, large specific surface area, acid and alkali resistance, high thermal stability, and environmental friendliness, so it is widely used in industrial fields such as adsorption, catalysis, and loading (Shen Zengmin et al., 2008). Using natural and synthetic porous materials as templates, templated porous carbons with different pore structures can be prepared. Among them, zeolite template carbon is mainly composed of microporous (pore diameter < 2nm) structure (Kyotani et al., 2003), while MCM-41 template carbon mainly contains mesoporous (pore diameter ≤ 50nm) structure (Liang et al., 2008) . However, the above-mentioned template carb...

Claims

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Application Information

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IPC IPC(8): C01B31/02C01B32/05
Inventor 刘冬袁鹏于文彬袁巍巍谭道永何宏平
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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