CN111960415B - Method for preparing granular activated carbon from coal semicoke - Google Patents
Method for preparing granular activated carbon from coal semicoke Download PDFInfo
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- CN111960415B CN111960415B CN202010827282.8A CN202010827282A CN111960415B CN 111960415 B CN111960415 B CN 111960415B CN 202010827282 A CN202010827282 A CN 202010827282A CN 111960415 B CN111960415 B CN 111960415B
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- C01B32/00—Carbon; Compounds thereof
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- C01B32/312—Preparation
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- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/336—Preparation characterised by gaseous activating agents
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- C—CHEMISTRY; METALLURGY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
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Abstract
The invention relates to a preparation method of activated carbon, which comprises the following steps: a pretreatment step, namely preparing a coal semicoke raw material into semicoke particles, and preparing granular mixtures of the semicoke particles and potassium carbonate; an activation step, namely heating the granular mixture obtained in the pretreatment step to a preset temperature T under the protection of inert gas, and activating the granular mixture in a water vapor environment; and a post-treatment step, namely, carrying out acid washing and drying on the granular mixture treated by the activation step to obtain granular activated carbon. The preparation method of the activated carbon provided by the invention adopts a process of combined activation of physical activation and chemical activation, so that not only can the energy consumption be reduced, but also the consumption of a chemical activating agent can be greatly reduced, the corrosivity to equipment is reduced, the maintenance cost of the equipment is reduced, and the quality of the activated carbon can be ensured.
Description
Technical Field
The invention relates to the technical field of carbon material preparation, in particular to a method for preparing granular activated carbon from coal semicoke.
Background
In recent years, in the fields of flue gas treatment, wastewater purification and the like, an adsorption method is widely applied due to the characteristics of simple operation and low cost. Among them, activated carbon is attracting attention as a solid adsorbent having stable physicochemical properties and excellent adsorption performance. The raw materials for preparing the activated carbon are from various sources, such as organic materials of coal, fruit shells, wood and the like. Compared with other raw materials, China has abundant coal resources, the concentrated development yield is huge, the coal semicoke obtained in the coal conversion process is low in price, the coal semicoke is often directly combusted, and the coal semicoke is discarded at will even as waste in some places, so that the environment is greatly influenced. The coal semi-coke has a certain pore structure, and then is subjected to a certain activation process, so that an activated carbon product with a developed pore structure and a certain economic value can be obtained.
The existing activated carbon preparation process generally comprises the process steps of pretreatment, carbonization, activation, post-treatment and the like, wherein various chemical reagents can be used, and certain environmental problems are caused. The main purpose of the carbonization process is to develop a main pore structure, and the reaction conditions of the pyrolysis process and the carbonization process of the semi-coke raw material are similar, so that the consumption of the process can be reduced, and the carbonization process is an ideal raw material for preparing the activated carbon. In addition, in the conventional activation process, physical activation or chemical activation is generally used alternatively. The physical activation temperature is generally higher, the time consumption is longer, and the energy consumption is larger; the activated carbon obtained by chemical activation has a developed pore structure, but the consumption of the activating agent is high, the activated carbon has strong corrosivity on equipment, and the large-scale production of the activated carbon is difficult.
Therefore, there is a need for an improved method of preparing activated carbon.
Disclosure of Invention
The invention provides a preparation method of granular activated carbon by adopting a physical and chemical combined activation process, aiming at reducing energy consumption, greatly reducing consumption of a chemical activating agent and reducing corrosion of the chemical activating agent to activation equipment.
In order to achieve the above object, the present invention provides a method for preparing granular activated carbon from coal semicoke, comprising the steps of:
a pretreatment step, namely preparing a coal semicoke raw material into semicoke particles, and preparing granular mixtures of the semicoke particles and potassium carbonate;
an activation step, namely heating the granular mixture obtained in the pretreatment step to a preset temperature T under the protection of inert gas, and activating the granular mixture in a water vapor environment; and
and a post-treatment step, namely, carrying out acid washing and drying on the mixture treated in the activation step to obtain the granular activated carbon.
In the technical scheme, the potassium carbonate and the semicoke particles are used for chemical activation, and compared with potassium hydroxide generally selected in the prior art, the potassium carbonate is weak in corrosivity and low in cost, so that the maintenance cost of activation equipment is reduced, the use cost is reduced, and the activated carbon can be produced in a large scale.
Meanwhile, the preparation method of the activated carbon provided by the invention adopts a process of combined activation of physical activation and chemical activation, so that not only can the energy consumption be reduced, but also the consumption of a chemical activating agent (potassium carbonate) can be greatly reduced, the production cost and the equipment maintenance cost are further reduced, and the quality of the activated carbon can be ensured.
In the preferred technical scheme of the invention, the preset temperature T is within the range of 750-850 ℃.
The existing physical activation process has high requirements on the activation temperature, usually at 900-. In addition, 750 ℃ and 850 ℃ are the preferred temperature range, and if the temperature is too high, the yield of the activated carbon product is reduced, and the product performance is influenced.
In the preferred technical scheme of the invention, in the activation step, the temperature rise rate ranges from 5 ℃ to 20 ℃/min.
In the technical scheme, the temperature rising rate ranges from 5 ℃ to 20 ℃/min, so that the phenomenon that the pore structure of the semicoke is damaged due to too fast temperature rise can be avoided, the temperature rising efficiency is ensured, and the energy waste is reduced.
In a preferred embodiment of the invention, the mass ratio of potassium carbonate to semicoke particles in the mixture in the pre-treatment step is 0.1-0.5.
In the technical scheme, the mass ratio of the potassium carbonate to the semicoke particles is 0.1-0.5. The content of potassium carbonate should not be too high, which would result in a decrease in yield. Preferably, the potassium carbonate is uniformly mixed with the particles by using an impregnation mode, so that excessive local activation is avoided, and the yield of the activated carbon product is reduced.
In the preferred technical scheme of the invention, in the activation step, the mass ratio of the water vapor is 0.6-1.5.
In the technical scheme, the mass ratio of the water vapor refers to the mass ratio of the water vapor participating in the activation reaction to the semicoke, and the water vapor with certain mass is uniformly introduced into the activation furnace in the activation reaction process. For example, the actual steam flow is 1.2kg/h under the reaction condition that the semicoke is 1kg, the steam mass ratio is 1.2 and the activation time is 1 hour. The range of the water vapor mass ratio is set to 0.6 to 1.5 because below this range, the activation reaction pore-enlarging effect is limited, and above this range, the yield of the activated carbon is lowered, and the performance of the activated carbon is affected.
In the preferred technical scheme of the invention, in the activation step, after the water vapor is introduced, the activation time is 0.5-1.5 h.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing activated carbon according to an embodiment of the present invention;
fig. 2 is a schematic material conveying line of an activated carbon preparation system according to an embodiment of the present invention.
Description of reference numerals:
1-a crusher;
2-dipping pool;
3-a dryer;
4-activating furnace;
5-acid washing tank.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the present embodiment provides a method for preparing activated carbon, including the steps of:
s1, a pretreatment step, namely preparing a coal semicoke raw material into semicoke particles, and preparing granular mixtures of the semicoke particles and potassium carbonate; s2 activation, namely heating the pretreated particles to a preset temperature T under the protection of inert gas, and introducing water vapor for activation; and S3 post-treatment step, namely, carrying out acid washing and drying on the mixture treated in the activation step to obtain the granular activated carbon.
In the embodiment, the potassium carbonate and the semi-coke particles are used for chemical activation, and compared with the potassium hydroxide generally selected in the prior art, the potassium carbonate is weak in corrosivity and low in cost, so that the maintenance cost of the activation equipment is reduced, the use cost is reduced, and the activated carbon can be produced in a large scale.
Meanwhile, the preparation method of the activated carbon provided by the embodiment adopts a process of combined activation of physical activation and chemical activation, so that not only can energy consumption be reduced, but also consumption of a chemical activating agent (potassium carbonate) can be greatly reduced, production cost and equipment maintenance cost are further reduced, and the quality of the activated carbon can be ensured.
Fig. 2 is a schematic material conveying line of an activated carbon preparation system according to an embodiment of the present invention. In the pretreatment step, the crusher 1 is adopted for crushing and screening to obtain semi-coke particles with a certain particle size, and in the embodiment, the particles with the diameter of 0.9-2mm (10-20 meshes) are screened out so as to fully activate the semi-coke raw material and facilitate the direct application of an activated carbon product.
Further, after the screened semicoke particles and potassium carbonate with a certain mass ratio are subjected to impregnation treatment in an impregnation tank 2, the semicoke particles are fed into a dryer 3 to be fully dried to remove moisture, then the dried semicoke and potassium carbonate mixture is fed into an activation furnace 4 to be subjected to combined activation of physical activation and chemical activation, and after the activation, the semicoke particles are subjected to acid washing in an acid washing tank 5, and finally the semicoke particles are dried in the dryer 3 to obtain the activated carbon.
Wherein, the semicoke particles and the potassium carbonate need to be fully impregnated, the impregnation time is 12 hours in the example, so that the semicoke and the potassium carbonate are fully mixed, and then the impregnated semicoke is fully dried to remove redundant moisture and avoid interfering with subsequent activation reaction.
After the impregnated particles enter the activation furnace 4, inert gas (such as nitrogen) is introduced into the activation furnace 4 as protective gas, purging is carried out for about 10min, the temperature is raised to the activation temperature of 750 and 850 ℃ at the speed of 5-20 ℃/min, and after the activation temperature is reached, water vapor is introduced into the activation furnace 3, so that the combined activation of physical activation and chemical activation is realized.
Wherein, the acid washing tank 5 can adopt acid solution such as dilute hydrochloric acid to carry out acid washing, and then the activated carbon after acid washing is washed to be neutral.
In the present embodiment, the range of the water vapor mass ratio is set to 0.6 to 1.5 because, when below this range, the activation reaming effect of the semicoke particles is limited and the product performance is poor; above this range, the yield of the activated carbon product is lowered, and the performance of the activated carbon product is affected.
Specifically, the mass ratio of water vapor refers to the mass ratio of water vapor participating in the activation reaction to semicoke, and a certain mass of water vapor is uniformly introduced into the activation furnace during the activation reaction. For example, the actual steam flow is 1.2kg/h under the reaction condition that the semicoke is 1kg, the steam mass ratio is 1.2 and the activation time is 1 hour.
In an embodiment, in the activation step, the combined activation is carried out for 0.5 to 1.5 hours after the introduction of water vapor. This is because, when it is less than this range, the activation effect of the semicoke particles is limited and the product properties are poor; above this range, over-activation, lower yields, and performance of the activated carbon product are affected.
The existing physical activation process has high requirements on the activation temperature, usually at 900-.
In the embodiment, the temperature rise rate ranges from 5 ℃/min to 20 ℃/min, and the phenomenon that the pore structure of the product is damaged due to too fast temperature rise can be avoided.
In this embodiment, the mass ratio of the potassium carbonate to the particles is 0.1 to 0.5.
It should be noted that, preferably, the ash content of the selected semicoke raw material in the embodiment is in a range of 10 to 30%, when the ash content is too high, the formation of a pore structure is affected, and when the ash content is too low, the requirement on raw coal is high, and the production cost is increased; on the other hand, certain ash removed in the acid washing process is beneficial to forming a new pore structure and improving the performance of the activated carbon, and correspondingly, the requirement on the quality of the raw material is too high due to too low ash content, and the cost is increased.
An embodiment is that: fully soaking 10-20 mesh coal semi-coke particles obtained by crushing and screening and potassium carbonate powder with the mass ratio of 0.2 for 12 hours, and drying for 4 hours at 120 ℃. Sending the pretreated particles into an activation furnace, heating to 800 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, and jointly activating for 1 hour under the working conditions of an activation temperature of 800 ℃ and a water vapor mass ratio of 1.2. Cooling to normal temperature, washing with dilute hydrochloric acid, and drying to obtain the active carbon product. The yield of the activated carbon product is 47.1 percent, and the specific surface area is 671.7m2The iodine value is 825.9mg/g, and the phenol adsorption value is 105.2 mg/g. Besides being applied to pollutant adsorption in water, the product also has good effect of being used for flue gas desulfurization and can be used for SO2The adsorbed amount was 31.2 mg/g.
Example two: fully soaking 10-20 mesh coal semi-coke particles obtained by crushing and screening with potassium carbonate powder with the mass ratio of 0.3 for 12 hours, and drying at 120 ℃ for 4 hours. Sending the pretreated particles into an activation furnace, heating to 750 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, and jointly activating for 1 hour under the working conditions of the activation temperature of 750 ℃ and the mass ratio of water vapor of 0.9. Cooling to normal temperature, washing with dilute hydrochloric acid, and drying to obtain the active carbon product. The yield of the activated carbon product is 62.0 percent, the iodine value is 730.9mg/g, and the phenol adsorption value is 72.2 mg/g.
Embodiment (c): fully soaking 10-20 mesh coal semi-coke particles obtained by crushing and screening with potassium carbonate powder with the mass ratio of 0.1 for 12 hours, and drying at 120 ℃ for 4 hours. Sending the pretreated particles into an activation furnace, heating to 800 ℃ at a heating rate of 10 ℃/min under the protection of nitrogen, and jointly activating for 1.5 hours under the working conditions of an activation temperature of 800 ℃ and a water vapor mass ratio of 0.9. Cooling to normal temperature, washing with dilute hydrochloric acid, and drying to obtain the active carbon product. The yield of the activated carbon product is 52.0 percent, the iodine value is 667.7mg/g, and the phenol adsorption value is 90.4 mg/g.
In some embodiments, the particles of coal char feedstock may also be mixed with the particles of potassium carbonate using mechanical mixing, followed by combined activation.
Example iv: fully mixing 10-20 mesh coal semi-coke particles obtained by crushing and screening with potassium carbonate powder with the mass ratio of 0.3, sending the mixture into an activation furnace, raising the temperature to 800 ℃ at the heating rate of 10 ℃/min under the protection of nitrogen, and jointly activating for 1 hour under the working conditions of the activation temperature of 800 ℃ and the mass ratio of water vapor of 1.2. Cooling to normal temperature, washing with dilute hydrochloric acid, and drying to obtain the active carbon product. The yield of the activated carbon product is 43.6 percent, and the specific surface area is 413.6m2(ii)/g, iodine value 425.1 mg/g.
It will be appreciated by those of ordinary skill in the art that in the embodiments described above, numerous technical details are set forth in order to provide a better understanding of the present application. However, the technical solutions claimed in the claims of the present application can be basically implemented without these technical details and various changes and modifications based on the above-described embodiments. Accordingly, in actual practice, various changes in form and detail may be made to the above-described embodiments without departing from the spirit and scope of the invention.
Claims (5)
1. The method for preparing the granular activated carbon by using the coal semicoke is characterized by comprising the following steps of:
a pretreatment step, namely preparing a coal semicoke raw material into semicoke particles, wherein the diameter of the semicoke particles is 0.9-2mm, and preparing granular mixtures from the semicoke particles and potassium carbonate; the mass ratio of the potassium carbonate to the semi-coke particles is 0.1-0.5; the ash content of the semicoke raw material is 10-30%;
an activation step, namely heating the granular mixture obtained in the pretreatment step to a preset temperature T under the protection of inert gas, and activating the granular mixture in a water vapor environment; in the activation step, the temperature rise rate ranges from 5 to 20 ℃/min; the activation time is 0.5-1.5 h; and
and a post-treatment step, namely performing acid washing and drying on the granular mixture treated in the activation step to obtain granular activated carbon.
2. The method for preparing granular activated carbon from coal semicoke as claimed in claim 1, wherein the predetermined temperature T is in the range of 750-850 ℃.
3. The method for preparing granular activated carbon from coal semicoke according to claim 1, wherein the pretreatment step comprises,
preparing a coal semicoke raw material into semicoke particles, soaking the semicoke particles with potassium carbonate, and drying to obtain the granular mixture.
4. The method for preparing granular activated carbon from coal semicoke according to claim 1, wherein the pretreatment step comprises,
the coal semicoke raw material is made into semicoke particles, and the semicoke particles are mechanically mixed with potassium carbonate to obtain the granular mixture.
5. The method for preparing granular activated carbon from coal semicoke according to claim 1, wherein in the activation step, the mass ratio of water vapor is 0.6-1.5.
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