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Spherical active carbon and preparation method thereof

A spherical activated carbon, activated technology, applied in the direction of chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve problems such as adhesion, different reaction progress, and specific surface area reduction, and reduce the chance of contact adhesion and particle size distribution Uniform, specific surface area reduction effect

Active Publication Date: 2019-12-20
CHINA SHENHUA COAL TO LIQUID & CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the current spherical activated carbon preparation method, for example, CN101143720A discloses a method for preparing activated carbon microsphere adsorption material after thermal condensation into spheres, but the mesophase microspheres formed by thermal condensation into spheres are difficult to separate from the solvent, and It is easy to stick together during the process, resulting in a decrease in sphericity, and the final prepared activated carbon has poor sphericity and small specific surface area.
CN103693641A discloses a method for preparing spherical activated carbon with water-soluble pitch. In order to avoid material coking and blocking the nozzle at the nozzle, it needs to be granulated by low-temperature spraying, and then carbonized and activated. However, due to the low temperature of pitch forming, carbonization and activation The process is longer, resulting in partial cracking and adhesion of the final spherical activated carbon
In other processes for preparing spherical activated carbon from pitch, external heat sources are generally used in the heat treatment process. Due to the transfer of heat from the outside to the inside and the transfer of the volatilized gas from the inside to the outside, the temperature is uneven, the reaction progress of the inside and outside of the material is different, and the inside of the material is rigid. When the reaction starts to produce pores, the external reaction of the material is excessive, which causes the pores to expand or even collapse, the specific surface area is reduced, the reaction time is prolonged, and it is not conducive to industrial production.

Method used

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  • Spherical active carbon and preparation method thereof

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preparation example Construction

[0038] The preparation method of the spherical activated carbon provided by the first aspect of the present invention, the method may further comprise the steps:

[0039] (1) mixing sulfonated asphalt with an activator, and spraying and granulating the obtained mixed solution to obtain mixed microspheres;

[0040] (2) microwave activation of the mixed microspheres to obtain active microspheres;

[0041] (3) removing impurities from the activated microspheres to obtain spherical activated carbon;

[0042] Wherein, the activator is potassium hydroxide, and the temperature of the spray granulation is 600-1000°C.

[0043] Preferably, the spray granulation temperature is 700-900°C, specifically 700°C, 750°C, 800°C, 850°C or 900°C.

[0044] In the present invention, by using potassium hydroxide as an activator, and carrying out spray granulation under the above conditions, the spray granulation can quickly obtain mixed microspheres, and the mixed microspheres have a better treatme...

Embodiment l

[0061] After the coal liquefied pitch and coking wash oil are mixed uniformly according to the weight ratio of 1:2, concentrated sulfuric acid is added dropwise to it for sulfonation reaction. The weight ratio of concentrated sulfuric acid and coal liquefied pitch is 1:4, and the sulfonation reaction temperature is 40°C, the sulfonation reaction time is 100min.

[0062] After the reaction is completed, the product of the above sulfonation reaction is neutralized with a KOH solution having a concentration of 40% by weight to obtain sulfonated pitch. The weight ratio of sulfonated asphalt and activator (KOH) is 1:1 to obtain sulfonated asphalt mixture.

[0063] Raise the temperature of the sulfonated asphalt mixture to 90°C, and spray it into the spray tower through a nozzle hole with a diameter of 1 mm at a pressure of 1.0 MPa. Under the protection of nitrogen, the droplets formed by spraying were rapidly pyrolyzed into mixed microspheres in the spray tower at 800 °C. The mix...

Embodiment 2-17、 comparative example 1-4

[0066] According to the method described in Example 1, the difference is that the preparation method was adjusted according to the parameters shown in Table 1. The properties of the final spherical activated carbon are shown in Table 1.

[0067] Table 1

[0068]

[0069] Method (1): Raise the temperature to 600°C for 1 hour at a heating rate of 1°C / min, then raise the temperature to 800°C for 1 hour at a heating rate of 2°C / min.

[0070] It can be seen from the results in Table 1 that the preparation of spherical activated carbon by the embodiment of the present invention has obvious advantages such as large specific surface area, simple process, and fast preparation speed.

[0071] In addition, it can be seen from the observation of the scanning electron microscope that the spherical activated carbon of the embodiment has good sphericity and uniform particle size distribution, which shows that the preparation method of the present invention has significantly better effect...

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Abstract

The invention relates to the field of active carbon preparation, and discloses spherical active carbon and a preparation method thereof. The method comprises the following steps: (1) mixing sulfonatedasphalt and an activating agent, and carrying out spray granulation on the obtained mixed solution to obtain mixed microspheres; (2) carrying out microwave activation on the mixed microspheres to obtain active microspheres; and (3) removing impurities from the active microspheres to obtain spherical active carbon, wherein the activating agent is potassium hydroxide, and the temperature of spray granulation is 600-1000 DEG C. The preparation method is simple and rapid, and the prepared spherical active carbon has the advantages of good sphericity, large specific surface area, uniform and controllable pore diameter, uniform particle size distribution and excellent adsorption performance.

Description

technical field [0001] The invention relates to the field of activated carbon preparation, in particular to a spherical activated carbon and a preparation method thereof. Background technique [0002] Spherical activated carbon has a series of advantages such as large specific surface area, fast adsorption and desorption speed, good sphericity, uniform packing density, high strength, and corrosion resistance. , environmental protection, military and other fields have broad application prospects. [0003] In the current spherical activated carbon preparation method, for example, CN101143720A discloses a method for preparing activated carbon microsphere adsorption material after thermal condensation into spheres, but the mesophase microspheres formed by thermal condensation into spheres are difficult to separate from the solvent, and It is easy to stick together during the treatment process, resulting in a decrease in sphericity, and the final prepared activated carbon has po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/348C01B32/33
CPCC01B32/33C01B32/348
Inventor 辛凡文李克健舒歌平向柠王洪学高山松杨葛灵程时富吴剑平曹利军
Owner CHINA SHENHUA COAL TO LIQUID & CHEM CO LTD
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