CN110589824A - Spherical activated carbon and preparation method thereof - Google Patents
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- CN110589824A CN110589824A CN201910828648.0A CN201910828648A CN110589824A CN 110589824 A CN110589824 A CN 110589824A CN 201910828648 A CN201910828648 A CN 201910828648A CN 110589824 A CN110589824 A CN 110589824A
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- C01B32/33—Preparation characterised by the starting materials from distillation residues of coal or petroleum; from petroleum acid sludge
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The invention relates to the field of activated carbon preparation, and discloses spherical activated carbon and a preparation method thereof. The method comprises the following steps: (1) mixing sulfonated asphalt with an activating agent, and performing spray granulation on the obtained mixed solution to obtain mixed microspheres; (2) performing microwave activation on the mixed microspheres to obtain active microspheres; (3) removing impurities from the active microspheres to obtain spherical active carbon; wherein the activating agent is potassium hydroxide, and the temperature of the spray granulation is 600-1000 ℃. The preparation method is simple and quick, and the prepared spherical activated 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
The invention relates to the field of activated carbon preparation, and particularly relates to spherical activated carbon and a preparation method thereof.
Background
The spherical activated carbon has a series of advantages of large specific surface area, high adsorption and desorption speed, good sphericity, uniform loading density, high strength, corrosion resistance and the like, can replace the conventional activated carbon and be applied to the traditional field, and has wide application prospects in the fields of electronics, biomedicine, environmental protection, military and the like.
In the current methods for preparing spherical activated carbon, for example, CN101143720A discloses a method for preparing an activated carbon microsphere adsorption material by thermal polycondensation and activation after balling, but the mesophase microspheres formed by the thermal polycondensation and balling method are difficult to separate from the solvent, and easily stick during the treatment process, resulting in reduced sphericity, and the finally prepared activated carbon has poor sphericity and small specific surface area. CN103693641A discloses a method for preparing spherical activated carbon by water-soluble asphalt, which is to avoid the blockage of the nozzle by coking of materials at the nozzle, and needs to be carbonized and activated after low-temperature spray granulation, but the final spherical activated carbon is partially cracked and adhered due to the long carbonization and activation process caused by the low temperature of the asphalt balling. In other processes for preparing spherical activated carbon from asphalt, an external heat source is generally adopted in the heat treatment process, and due to the fact that heat is transferred from outside to inside and gas volatilized by reaction is transferred from inside to outside, the temperature is not uniform, the inside and outside reaction progress of materials is different, when pores are generated by the reaction just beginning in the materials, the external reaction of the materials is excessive, so that the pores are expanded or even collapsed, the specific surface area is reduced, the reaction time is prolonged, and the problems of industrial production are solved.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide spherical activated carbon and a preparation method thereof.
In order to achieve the above objects, one aspect of the present invention provides a method for preparing spherical activated carbon, the method comprising the steps of:
(1) mixing sulfonated asphalt with an activating agent, and performing spray granulation on the obtained mixed solution to obtain mixed microspheres;
(2) performing microwave activation on the mixed microspheres to obtain active microspheres;
(3) removing impurities from the active microspheres to obtain spherical active carbon;
wherein the activating agent is potassium hydroxide, and the temperature of the spray granulation is 600-1000 ℃.
Preferably, the sulfonated asphalt is obtained by uniformly mixing an asphalt raw material with an organic solvent and then carrying out sulfonation reaction with a sulfonating agent.
Preferably, the asphalt raw material is one or more of coal liquefied asphalt, petroleum asphalt, coal coking asphalt and natural asphalt.
Preferably, the organic solvent is at least one of coker wash oil, tetrahydrofuran, carbon tetrachloride, coal-liquefied light oil, and petroleum middle distillate.
Preferably, the weight ratio of the asphalt feedstock to the organic solvent is 1: 2-8.
Preferably, the sulfonating agent is oleum and/or concentrated sulfuric acid.
Preferably, the weight ratio of the asphalt raw material to the sulfonating agent is 1: 0.2-1.
Preferably, the sulfonation reaction conditions include: the temperature is 20-45 deg.C, and the time is 30-400 min.
Preferably, the weight ratio of the sulfonated asphalt to potassium hydroxide is 1: 0.2-1.5, more preferably 1: 0.2 to 1.2, more preferably 1: 0.5-1.2.
Preferably, the activator is mixed with the sulfonated asphalt as a solid and/or as an aqueous solution.
Preferably, the aqueous activator solution has a concentration of 30 to 50 wt.%.
Preferably, the diameter of the spray hole of the spray is 0.3-1mm, and the feeding pressure of the spray nozzle is controlled to be 0.1-2 MPa.
Preferably, the spray is direct from top to bottom.
Preferably, the temperature of the mixture of sulfonated asphalt and activator before spraying is 80-95 ℃.
Preferably, the height of the spray tower is 2-6m and the diameter is 1-3 m.
Preferably, the power of the microwave activation is 500-1500W.
Preferably, the microwave activation time is 5-20 min.
Preferably, the microwave activation is performed in a nitrogen or inert gas atmosphere.
Preferably, the removing impurities comprises: mixing the active microspheres with acid and boiling.
Preferably, the acid is 4-10% nitric acid by mass.
Preferably, the method further comprises the steps of adjusting the pH value of the boiled solution to 6-7, and then sequentially carrying out solid-liquid separation, washing and drying to obtain the spherical activated carbon.
The second aspect of the present invention provides the spherical activated carbon prepared by the above-mentioned preparation method of the present invention.
Preferably, the specific surface area of the spherical activated carbon is 2300m2More than g.
Through the technical scheme, the spherical activated carbon prepared by the invention has the advantages of high preparation speed, good sphericity, large specific surface area, uniform and controllable pore diameter, uniform particle size distribution and excellent adsorption performance, and is mainly characterized in the following aspects:
(1) the mixed microsphere is prepared in a high-temperature spray pyrolysis balling mode, light components such as a solvent and the like are separated out after being changed into a gaseous state in the spraying process, the mixed microsphere can keep better sphericity in the carbonization and activation processes, and the problems of fusion adhesion and deformation of the microsphere caused by the fact that part of the light components are remained in the microsphere due to low temperature in the traditional spray balling process are solved.
(2) Adopt outer heat source in the conventional activated carbon preparation process, cause the temperature inhomogeneous, the inside and outside reaction progress of material is different, when just beginning to react and produce the hole in the material is inside, the outside reaction of material is excessive to cause the hole expansion to collapse even, also do not benefit to the problem of industrial production when specific surface area reduces, reaction time extension. The invention utilizes the advantages of microwave which can directly heat the interior of the material, uniform heating, high speed and the like, and combines the characteristic of good intersolubility of the sulfonated asphalt and the activating agent, so that a large amount of active points can be generated in the interior of the mixed microsphere, the activation temperature is reduced, the preparation process of the activated carbon is less in use, the activation process is controllable, and the energy consumption is low.
(3) The mixed microspheres formed by spraying in the invention are subjected to microwave activation through a microwave field in the process of free falling, so that the contact adhesion between the microspheres is reduced, the reaction is more uniform, and the formed activated carbon has uniform particle size distribution and controllable pore size.
(4) The invention has simple production process, timely operation and control and small pollution, and is suitable for industrial continuous production.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The preparation method of the spherical activated carbon provided by the first aspect of the invention comprises the following steps:
(1) mixing sulfonated asphalt with an activating agent, and performing spray granulation on the obtained mixed solution to obtain mixed microspheres;
(2) performing microwave activation on the mixed microspheres to obtain active microspheres;
(3) removing impurities from the active microspheres to obtain spherical active carbon;
wherein the activating agent is potassium hydroxide, and the temperature of the spray granulation is 600-1000 ℃.
Preferably, the temperature of the spray granulation is 700-900 ℃, and specifically can be 700 ℃, 750 ℃, 800 ℃, 850 ℃ or 900 ℃, and the like.
In the invention, potassium hydroxide is used as an activating agent, and spray granulation is carried out under the conditions, so that the mixed microspheres can be quickly obtained by spray granulation, and the mixed microspheres have better treatment effect under the action of microwaves.
In the present invention, the sulfonated asphalt is an asphalt subjected to sulfonation treatment, and a commercially available sulfonated asphalt can be used, or the sulfonated asphalt can be prepared by the method of the present invention described below. The spherical activated carbon is preferably produced by the method of the present invention described below, from the viewpoint of improving the properties of the spherical activated carbon to be finally obtained.
According to a specific embodiment of the present invention, the sulfonated asphalt can be obtained by mixing asphalt raw material with organic solvent, and then sulfonating with sulfonating agent.
In the above preparation method, the asphalt raw material may be one or more of coal liquefied asphalt, petroleum asphalt, coal tar pitch and natural asphalt, and is preferably coal liquefied asphalt and/or petroleum asphalt. Specifically, the coal-liquefied asphalt may be asphalt obtained by direct liquefaction of coal or indirect liquefaction of coal; petroleum asphalt is asphalt obtained in the course of crude oil processing.
In addition, the organic solvent is at least one of coking wash oil, tetrahydrofuran, carbon tetrachloride, coal liquefaction light oil and petroleum middle distillate, and is preferably coking wash oil and/or carbon tetrachloride. Wherein the coking wash oil refers to wash oil meeting the standard of GB/T24217-2009 wash oil; the coal-to-liquid light oil refers to a fraction with the distillation range of 180-230 ℃ after coal liquefaction, and can be purchased from Shenhua coal oil chemical industry Co., Ltd, China, for example; the petroleum middle fraction refers to the fraction boiling at 200 ℃ and 250 ℃. In order to increase the efficiency of the sulfonation reaction, it is preferable that the weight ratio of the asphalt starting material to the organic solvent is 1: 2-8, more preferably 1: 2-4, more preferably 1: 2-3.
In the above production method, the sulfonating agent may be fuming sulfuric acid and/or concentrated sulfuric acid (a sulfuric acid solution having a mass fraction of 70% or more, preferably a sulfuric acid solution having a mass fraction of 98% or more). In order to increase the efficiency of the sulfonation reaction, preferably, the weight ratio of the asphalt starting material to the sulfonating agent is 1: 0.2 to 1, more preferably 1: 0.25-0.4. The conditions of the sulfonation reaction are not particularly limited as long as the sulfonation reaction can be carried out to obtain sulfonated asphalt, and preferably, the temperature of the sulfonation reaction is 20-45 ℃, preferably 30-40 ℃; the time is 30-400min, preferably 100-150 min.
In step (1) above, the activator may be mixed with the sulfonated asphalt in the form of a solid and/or an aqueous solution. When mixed in the form of an aqueous solution, the concentration of the aqueous activator solution is preferably 30 to 50% by weight, more preferably 45 to 45% by weight. Among them, it is preferable to mix in a solid form.
In the step (1), the weight ratio of the sulfonated asphalt to the potassium hydroxide is preferably 1: 0.2-1.5, more preferably 1: 0.2 to 1.2, more preferably 1: 0.5-1.2. By using potassium hydroxide as an activator in the above ratio, the specific surface area and pore volume of the resulting spherical activated carbon can be further increased.
In the step (1) above, the spray granulation may be performed using any spray granulator as long as the desired mixed microspheres can be obtained, and for example, the height of the spray tower may be 2 to 6m and the diameter may be 1 to 3 m. From the viewpoint of the properties of the spherical activated carbon to be produced, it is preferable that the diameter of the spray hole of the spray is 0.1 to 2mm, preferably 0.3 to 1mm, and the feed pressure of the nozzle is controlled to 0.1 to 2MPa, preferably 0.2 to 1MPa, more preferably 0.5 to 1 MPa. The spraying method is not particularly limited, but is preferably a method of direct spraying from top to bottom, and preferably microwave activation is performed simultaneously during the fall.
In order to enhance the effect of spray granulation, the temperature of the mixture of sulfonated asphalt and activator before spraying is preferably in the range of 80 to 95 deg.C, more preferably 85 to 90 deg.C.
In the step (2), the mixed microspheres obtained by spray granulation are subjected to microwave activation, so that the active microspheres are obtained. The conditions of the microwave activation are not particularly limited, and preferably include, from the viewpoint of the properties of the spherical activated carbon produced: the power is 500-1500W, preferably 800-1500W, more preferably 1200-1500W; preferably, the conditions of microwave activation include: the time is 5-20min, preferably 10-20 min; also, it is preferable that the microwave activation is performed in a nitrogen gas or inert gas atmosphere.
In the step (3), the active microspheres prepared by microwave activation are subjected to impurity removal to obtain spherical active carbon. The impurity removal is used for removing potassium hydroxide in the active microspheres and impurities generated by reaction of the potassium hydroxide. Preferably, the removing impurities comprises: mixing the active microspheres with acid and boiling. The acid used for the impurity removal is not particularly limited, and for example, sulfuric acid, nitric acid, or the like can be used, and preferably, the acid is nitric acid with a mass percentage of 4 to 10%.
Preferably, the method further comprises adjusting the pH value of the boiled solution to 6-7, and then sequentially carrying out solid-liquid separation, washing and drying to obtain the spherical activated carbon. Through the solid-liquid separation, washing and drying, impurities on the spherical activated carbon can be further removed. The solid-liquid separation is preferably carried out by filtration. Washing may be carried out more than 2 times, for example 3-5 times. The conditions for drying may include, for example: the temperature is 80-120 ℃ and the time is 3-12h, preferably, the temperature is 105-.
The second aspect of the present invention provides the spherical activated carbon prepared by the above-mentioned preparation method of the present invention. By using the above-mentioned method of the present invention, activated carbon having a larger specific surface area can be obtained, and the specific surface area can be 2500m, for example2More specifically,/g is not less than. The specific surface area can be measured by the BET method.
The present invention will be described in detail below by way of examples. In the following examples and comparative examples, the diameter was measured by a malvern laser particle size analyzer Mastersizer 3000, and the specific surface area and pore volume were measured by a BET method using a conatautosorb-iQ full-automatic specific surface and pore size distribution analyzer.
In the following examples and comparative examples, the coal-liquefied asphalt is a low ash asphalt product of Shenhua coal-to-liquids chemical industries, Ltd; the petroleum asphalt is east China sea 70# asphalt of Qilu petrochemical company.
Example l
Mixing coal liquefied asphalt and coking wash oil according to the weight ratio of 1: 2, after uniformly mixing, dropwise adding concentrated sulfuric acid into the mixture to perform sulfonation reaction, wherein the weight ratio of the concentrated sulfuric acid to the coal liquefaction asphalt is 1: and 4, controlling the sulfonation reaction temperature to be 40 ℃ and the sulfonation reaction time to be 100 min.
And after the reaction is finished, neutralizing the product of the sulfonation reaction by using a KOH solution with the concentration of 40 weight percent to obtain the sulfonated asphalt. Mixing the sulfonated asphalt and an activating agent (KOH) in a weight ratio of 1: 1, obtaining a sulfonated asphalt mixed solution.
Heating the sulfonated asphalt mixed solution to 90 ℃, and spraying the sulfonated asphalt mixed solution into a spraying tower through a spray hole with the diameter of 1mm under the pressure of 1.0 MPa. Under the protection of nitrogen, the liquid drops formed by spraying are quickly pyrolyzed into mixed microspheres in a spray tower at 800 ℃. And (3) performing high-temperature activation on the mixed microspheres for 20min by using a 1200W microwave field to obtain activated microspheres.
After cooling, the activated microspheres were washed with an excess of 8% HNO by mass3The properties of the spherical activated carbon obtained after washing with water, boiling, washing with water to a pH of 7, filtration and drying (105 ℃ C., 6h) are shown in Table 1.
Examples 2 to 17, comparative examples 1 to 4
The procedure is as described in example 1, except that the preparation is adjusted according to the parameters indicated in Table 1. The properties of the finally obtained spherical activated carbon are shown in table 1.
TABLE 1
Method (1): the temperature is raised to 600 ℃ at the heating rate of 1 ℃/min for carbonization for 1h, and then the temperature is raised to 800 ℃ at the heating rate of 2 ℃/min for activation for 1 h.
As can be seen from the results in Table 1, the spherical activated carbon prepared by the embodiment of the invention has the obvious advantages of large specific surface area, simple process, high preparation speed and the like.
In addition, the observation of a scanning electron microscope shows that the spherical activated carbon of the embodiment has good sphericity and uniform particle size distribution, which shows that the preparation method of the invention has obviously better effect compared with the existing method.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for preparing spherical activated carbon is characterized by comprising the following steps:
(1) mixing sulfonated asphalt with an activating agent, and performing spray granulation on the obtained mixed solution to obtain mixed microspheres;
(2) performing microwave activation on the mixed microspheres to obtain active microspheres;
(3) removing impurities from the active microspheres to obtain spherical active carbon;
wherein the activating agent is potassium hydroxide, and the temperature of the spray granulation is 600-1000 ℃.
2. The preparation method according to claim 1, wherein the sulfonated asphalt is obtained by mixing an asphalt raw material with an organic solvent, and then performing sulfonation with a sulfonating agent.
3. The preparation method according to claim 2, wherein the asphalt raw material is one or more of coal liquefied asphalt, petroleum asphalt, coal tar pitch and natural asphalt;
preferably, the organic solvent is at least one of coker wash oil, tetrahydrofuran, carbon tetrachloride, coal liquefaction light oil and petroleum middle distillate;
preferably, the weight ratio of the asphalt feedstock to the organic solvent is 1: 2-8.
4. The production method according to claim 2, wherein the sulfonating agent is fuming sulfuric acid and/or concentrated sulfuric acid;
preferably, the weight ratio of the asphalt raw material to the sulfonating agent is 1: 0.2 to 1;
preferably, the sulfonation reaction conditions include: the temperature is 20-45 deg.C, and the time is 30-400 min.
5. The method of any of claims 1-4, wherein the weight ratio of sulfonated asphalt to potassium hydroxide is 1: 0.2-1.5, more preferably 1: 0.2 to 1.2, more preferably 1: 0.5-1.2;
preferably, the activator is mixed with the sulfonated asphalt as a solid and/or as an aqueous solution;
preferably, the aqueous activator solution has a concentration of 30 to 50 wt.%.
6. The method according to any one of claims 1 to 4, wherein the temperature of the spray granulation is 700-900 ℃;
preferably, the diameter of the spray hole of the spray is 0.3-1mm, and the feeding pressure of the spray nozzle is controlled to be 0.1-2 MPa;
preferably, the spray is direct spray from top to bottom;
preferably, the temperature of the mixture of sulfonated asphalt and activator before spraying is 80-95 ℃;
preferably, the height of the spray tower is 2-6m and the diameter is 1-3 m.
7. The preparation method according to any one of claims 1-4, wherein the power of the microwave activation is 500-1500W;
preferably, the microwave activation time is 5-20 min;
preferably, the microwave activation is performed in a nitrogen or inert gas atmosphere.
8. The production method according to any one of claims 1 to 4, wherein the impurity removal includes: mixing the active microspheres with acid and boiling;
preferably, the acid is 4-10% by mass of nitric acid;
preferably, the method further comprises the steps of adjusting the pH value of the boiled solution to 6-7, and then sequentially carrying out solid-liquid separation, washing and drying to obtain the spherical activated carbon.
9. Spherical activated carbon obtained by the production method according to any one of claims 1 to 8.
10. The spherical activated carbon as claimed in claim 9, wherein the spherical activated carbon has a specific surface area of 2300m2More than g.
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| CN113582159A (en) * | 2021-09-29 | 2021-11-02 | 天津师范大学 | High-capacitance porous carbon material and preparation method thereof |
| CN113716561A (en) * | 2021-07-14 | 2021-11-30 | 中国神华煤制油化工有限公司 | Preparation method of spherical activated carbon, spherical activated carbon and preparation device thereof |
| CN114408918A (en) * | 2022-02-15 | 2022-04-29 | 中国神华煤制油化工有限公司 | Asphalt-based hollow activated carbon microsphere, preparation method thereof, electrode slice and supercapacitor |
| CN114684817A (en) * | 2021-11-12 | 2022-07-01 | 中国神华煤制油化工有限公司 | Method and apparatus for preparing spherical negative active material, negative electrode for lithium battery, and lithium battery |
| CN114799184A (en) * | 2022-05-12 | 2022-07-29 | 江西咏泰粉末冶金有限公司 | Preparation method of high-uniformity large-particle spherical composite powder |
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| CN113716561A (en) * | 2021-07-14 | 2021-11-30 | 中国神华煤制油化工有限公司 | Preparation method of spherical activated carbon, spherical activated carbon and preparation device thereof |
| CN113582159A (en) * | 2021-09-29 | 2021-11-02 | 天津师范大学 | High-capacitance porous carbon material and preparation method thereof |
| CN114684817A (en) * | 2021-11-12 | 2022-07-01 | 中国神华煤制油化工有限公司 | Method and apparatus for preparing spherical negative active material, negative electrode for lithium battery, and lithium battery |
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| CN114408918A (en) * | 2022-02-15 | 2022-04-29 | 中国神华煤制油化工有限公司 | Asphalt-based hollow activated carbon microsphere, preparation method thereof, electrode slice and supercapacitor |
| CN114408918B (en) * | 2022-02-15 | 2023-10-13 | 中国神华煤制油化工有限公司 | Asphalt-based hollow activated carbon microsphere, preparation method thereof, electrode plate and supercapacitor |
| CN114799184A (en) * | 2022-05-12 | 2022-07-29 | 江西咏泰粉末冶金有限公司 | Preparation method of high-uniformity large-particle spherical composite powder |
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