CN111892050A - Preparation method for producing layered porous activated carbon with high specific surface area - Google Patents
Preparation method for producing layered porous activated carbon with high specific surface area Download PDFInfo
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- CN111892050A CN111892050A CN202010902504.8A CN202010902504A CN111892050A CN 111892050 A CN111892050 A CN 111892050A CN 202010902504 A CN202010902504 A CN 202010902504A CN 111892050 A CN111892050 A CN 111892050A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- 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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/39—Apparatus for the preparation thereof
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B17/00—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement
- F26B17/02—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement with movement performed by belts carrying the materials; with movement performed by belts or elements attached to endless belts or chains propelling the materials over stationary surfaces
- F26B17/04—Machines or apparatus for drying materials in loose, plastic, or fluidised form, e.g. granules, staple fibres, with progressive movement with movement performed by belts carrying the materials; with movement performed by belts or elements attached to endless belts or chains propelling the materials over stationary surfaces the belts being all horizontal or slightly inclined
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
- F26B23/04—Heating arrangements using electric heating
- F26B23/06—Heating arrangements using electric heating resistance heating
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
Abstract
The invention discloses a preparation method for producing layered porous activated carbon with high specific surface area, which comprises the steps of firstly crushing agricultural and forestry wastes (such as materials such as pericarp, straw, leaves or fermentation residues) and then carbonizing the crushed wastes for 1-5 hours at 600 ℃ in a nitrogen atmosphere, then mixing the crushed wastes with potassium hydroxide (the mass ratio is 1: 1-1: 6), then pretreating and drying the mixture at 70-100 ℃, transferring the dried mixture into a nickel crucible, activating the mixture for 1-4 hours at 500 ℃ in nitrogen, then heating the mixture to 1000 ℃ for carbonizing for 1-5 hours, washing the product with water, then using hydrochloric acid to leave inorganic salt, washing the product to be neutral, and then drying the black powder product; the invention has the following advantages: (1) the simple ethanol and potassium hydroxide pretreatment method is adopted, so that the method is suitable for large-scale industrial production; (2) the obtained material has ultrahigh specific surface area and porous structure; (3) the representative product has good electrochemical performance and adsorption capacity; in addition, the product has potential application value in the fields of electrode of super capacitor battery, drug carrier and pollutant removal.
Description
Technical Field
The invention belongs to the technical field of carbon materials, and particularly relates to a preparation method for producing layered porous activated carbon with high specific surface area.
Background
State-of-the-art electrochemical devices for energy storage, such as lithium ion batteries and Supercapacitors (SCs), have been widely used in electronic and electric vehicles. Compared to lithium ion batteries, SCs have a high power density: (>10kW kg-1) Excellent cycling stability and reliable safety, but limited energy density (5-10W h kg)-1). Different super capacitors are in types according to different energy storage mechanisms. Electrochemical Double Layer Capacitors (EDLCs) store energy by electrostatic adsorption of electrolyte ions at the electrode/electrolyte interface, thereby achieving rapid charge/discharge rates. Pseudocapacitors primarily utilize reversible faradaic reactions to provide higher capacitance and energy density than EDLCs. Different potential windows can obtain larger working voltage and provide higher energy density.
Multipurpose carbon materials such as Activated Carbon (ACS), graphene (graphene), Carbon Nanotubes (CNTs), and carbide-derived carbon have been widely studied as electrode materials for EDLCs. Many efforts have been made to improve their electrochemical performance. In particular, capacitance and rate performance are improved by increasing the Specific Surface Area (SSAs) of the carbon and adjusting the pore distribution of the carbon to provide more electroactive sites and ion transport pathways. The reasonable design of the nano structure can shorten the transport path of ions, so that the nano structure has good physical and chemical stability. The high graphitization degree ensures good conductivity and is beneficial to rapid ionic reaction at a high rate. The porous carbon with high specific surface area is generally used as an electrode material of a super capacitor due to the advantages of wide potential window, physical and chemical stability, easiness in preparation and the like.
At present, the active carbon is prepared by pyrolyzing and activating carbon-containing raw materials such as wood, coal, petroleum coke and the like, and the waste is effectively utilized and converted into renewable energy in the 21 st century with resource shortage, so that the sustainable development strategy of China is met; in some fields and countries, natural gas used by farmers and plant wastes generated in agricultural operation cannot be effectively and fully utilized, so that the plant wastes are rotted in soil, if the plant wastes can be utilized, on one hand, the existing waste gas resources are fully utilized, the utilization of other non-renewable resources is reduced, and on the other hand, the farmers sell the plant wastes to an activated carbon processing plant, and extra income can be brought.
Disclosure of Invention
In view of the above, the present invention provides a simple and practical method for preparing porous carbon particles with high specific surface area, so as to reduce production cost and achieve efficient utilization, and the obtained porous carbon particles with high specific surface area have good electrochemical energy storage performance and have application potential in the fields of supercapacitor electrodes, battery electrodes, drug carriers and pollutant removal.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method for producing layered porous activated carbon with high specific surface area comprises the following steps of pretreating activated carbon derived from forestry and agricultural residues at 70-100 ℃ by using ethanol and potassium hydroxide (mass ratio is 1: 1-6: 1), and then carrying out high-temperature pyrolysis combination under the atmosphere of protective gas such as nitrogen and argon to finally obtain the porous carbon particles with high specific surface area.
Preferably, in the pretreatment step, one or more of the mixture of the crushed pericarp, straw, leaves and fermentation residue agricultural and forestry waste is carbonized at 600 ℃ for 1-5 hours under nitrogen atmosphere, and then the mixture of ethanol and potassium hydroxide is pretreated in an oven at 70-100 ℃ after being mixed with the activated carbon according to a certain proportion.
Preferably, in the pretreatment step, one or more of the crushed pericarp, straw, leaves and fermentation residue agricultural and forestry waste is/are carbonized at 600 ℃ for 1-5 hours under nitrogen atmosphere to obtain plant activated carbon, then potassium hydroxide and 2g of activated carbon are mixed according to the mass ratio of 1:1, 2:1, 3:1, 4:1, 5:1 and 6:1 respectively, 50-100 ml of ethanol water solution with the volume ratio of 50%, 60%, 70%, 80% and 90% is added respectively, and after ultrasonic treatment is carried out for 30 minutes, the mixture is placed in an oven to be dried at 70-100 ℃.
Preferably, in the high-temperature pyrolysis combination step, the pretreated sample is placed in nitrogen gas, and is heated to 500 ℃ for activation for 1-4 hours at 300-.
Preferably, the high temperature pyrolysis combination step comprises placing the sample in nitrogen gas, raising the temperature to 500 ℃ at the rate of 5 ℃/min, activating for 1-4 hours, and raising the temperature to 1000 ℃ at the rate of 5 ℃/min, and carbonizing for 1-5 hours.
Preferably, after the carbonized sample is washed by pure water, residual inorganic salt is removed by hydrochloric acid, and then the sample is washed to be neutral by pure water, and vacuum drying is carried out at 80 ℃ to obtain the final porous carbon particles with high specific surface area.
Preferably, the carbonized sample is centrifugally washed to be neutral by pure water, then 50-100 ml of hydrochloric acid solution with the concentration of 1 mol per liter is added, the mixture is ultrasonically washed to be neutral by water after 30 minutes, and the mixture is placed into a vacuum drying oven at 80 ℃ to be dried for 12 hours to obtain the final porous carbon particles with high specific surface area.
Preferably, the oven used in the pretreatment step comprises a box body and a feeding box; a discharge port is formed in one side of the box body, and a conveying belt and a heating resistance wire are arranged in the box body; one end of the conveying belt is hinged at the discharge port, the other end of the conveying belt is hinged on the inner side wall of the box body, a heating resistance wire is arranged above the conveying belt and connected to the inner top surface of the box body, and the heating resistance wire is used for drying materials; a motor is arranged on the outer side wall of the lower half part in the feeding box; an output shaft of the motor extends into the feeding box, a roller is arranged on the output shaft, and an extrusion block is arranged on the surface of the roller; a discharge chute is arranged on one side of the lower half part of the feeding box, an entity is arranged on one side of the discharge chute, a groove is formed in the upper end of the entity, an extrusion block is arranged on the inner surface of the groove, and a cavity is arranged on one side of the entity; the end part of an output shaft of the motor is provided with a belt which is positioned in the cavity, and the end part of the output shaft of the motor is connected with the other end of the conveyor belt through the belt.
Preferably, a plurality of rows of bulges are uniformly arranged on the surface of the conveyor belt; a swing rod is arranged on the inner side of the discharge hole; one end of the swing rod is hinged to the inner wall of the box body, the middle position of the swing rod is connected to the inner side wall of the box body through a spring arranged on the inner wall of the box body, and the other end of the swing rod is located between two adjacent rows of bulges on the conveying belt.
Preferably, the heating resistance wire is fixedly connected to a connecting plate arranged in the box body; one end of the connecting plate is hinged to the inner top surface of the box body, and the other end of the connecting plate is provided with a push rod; the push rod runs through the arc-shaped holes symmetrically formed in the side wall of the box body, the part, located outside the box body, of the push rod is provided with a limiting rod, and two ends of the limiting rod are embedded into the fixing holes formed in two sides of the arc-shaped holes.
Compared with the prior art, the invention has the beneficial effects that:
the method comprises the steps of firstly, pre-carbonizing agricultural and forestry wastes such as fruit peels, straws, leaves or fermentation residues to obtain plant activated carbon, then, carrying out mixed pretreatment on the plant activated carbon by using ethanol and potassium hydroxide, and then, obtaining porous carbon particles with high specific surface area by utilizing high-temperature pyrolysis; the invention provides an important method which is simple, convenient, cheap and can be produced in large scale for preparing the porous carbon particles with ultrahigh specific surface area; the invention has the following advantages: (1) the simple ethanol and potassium hydroxide pretreatment method is adopted, so that the formation of the porous carbon particles with high specific surface area can be effectively promoted; (2) the prepared material has ultrahigh specific surface area and porosity; (3) the high-surface-area porous carbon particles synthesized by the method have good performance of electrode materials of the super capacitor and excellent electrochemical energy storage performance; in addition, the material has potential application value in lithium ion batteries, pollutant removal and other fields.
The plant wastes are utilized, on one hand, the existing waste gas resources are fully utilized, the utilization of other non-renewable resources is reduced, on the other hand, the plant wastes are sold to an active carbon processing factory by farmers, and extra income can be brought.
When the materials are subjected to drying intervention treatment in the drying oven, the materials are taken out of the groove by the roller wheel and flow onto the conveying belt along the discharging groove; when the motor rotates, the output shaft of motor passes through the electronic conveyer belt operation of belt, material flows to the conveyer belt on, then carries out drying process through the heat that the heating resistor silk produced, discharges from the discharge gate department of box at last, and this process is drying before the intervention processing to the material, and the material rolls the thin fragmentation once more, improves the mixed degree between the material simultaneously, improves material preliminary treatment's effect.
Drawings
FIG. 1 is a scanning electron microscope image of the porous carbon particles with high specific surface area prepared in example 1 of the present invention;
fig. 2 is a nitrogen adsorption/desorption curve and a pore size distribution curve of the porous carbon particles with high specific surface area prepared in example 1 of the present invention;
FIG. 3 is the electrochemical energy storage performance of the porous carbon particles with high specific surface area prepared in example 1 of the present invention in 6M KOH;
FIG. 4 is a perspective view of an oven of the present invention;
FIG. 5 is an enlarged view of a portion of FIG. 4 at A;
FIG. 6 is a cross-sectional view of an oven of the present invention;
FIG. 7 is an enlarged view of a portion of FIG. 6 at B;
FIG. 8 is an enlarged view of a portion of FIG. 6 at C;
in the figure: the device comprises a box body 1, a discharge hole 11, a swing rod 111, a spring 112, an arc-shaped hole 12, a fixing hole 121, a feeding box 2, a conveyor belt 3, a protrusion 31, a heating resistance wire 4, a connecting plate 41, a push rod 411, a limiting rod 412, a motor 21, a belt 211, a roller 22, an extrusion block 221, a discharge chute 23 and a groove 24.
Detailed Description
In order to further illustrate the present invention, the following description is given with reference to the examples and the accompanying drawings.
Example 1
As shown in fig. 1-3, the crushed fruit peels, straws, leaves or fermentation residues of agricultural and forestry waste are carbonized for 3 hours at 400 ℃ in a nitrogen atmosphere to obtain plant activated carbon; and then mixing 2g of plant activated carbon with 6g of potassium hydroxide according to the mass ratio of 1:3, adding 80 ml of ethanol solution with the volume fraction of 70%, carrying out ultrasonic treatment for 30 minutes, then putting the mixture into a 100-DEG C oven for drying, transferring the dried carbon sample into a nickel crucible, placing the nickel crucible into nitrogen for activation for 1.5 hours at 400 ℃, then heating to 900 ℃ for carbonization for 2 hours, cooling to room temperature, and washing the product with water and hydrochloric acid to obtain the high-surface-area porous carbon particles.
Example 2
As shown in fig. 1-3, the crushed fruit peels, straws, leaves or fermentation residues of agricultural and forestry waste are carbonized for 3 hours at 400 ℃ in a nitrogen atmosphere to obtain plant activated carbon; and then mixing 2g of plant activated carbon with 6g of potassium hydroxide according to the mass ratio of 1:3, adding 80 ml of ethanol solution with the volume fraction of 70%, carrying out ultrasonic treatment for 30 minutes, then putting the mixture into a 100-DEG C oven for drying, transferring the dried carbon sample into a nickel crucible, placing the nickel crucible into nitrogen for activation for 1.5 hours at 400 ℃, then heating to 800 ℃ for carbonization for 2 hours, cooling to room temperature, and washing the product with water and hydrochloric acid to obtain the porous carbon particles with high surface area.
Example 3
As shown in fig. 1-3, the crushed fruit peels, straws, leaves or fermentation residues of agricultural and forestry waste are carbonized for 3 hours at 400 ℃ in a nitrogen atmosphere to obtain plant activated carbon; and then mixing 2g of plant activated carbon with 6g of potassium hydroxide according to the mass ratio of 1:3, adding 80 ml of ethanol solution with the volume fraction of 70%, carrying out ultrasonic treatment for 30 minutes, then putting the mixture into a 100-DEG C oven for drying, transferring the dried carbon sample into a nickel crucible, placing the nickel crucible into nitrogen for activation for 1.5 hours at 400 ℃, then heating to 1000 ℃ for carbonization for 2 hours, cooling to room temperature, and washing the product with water and hydrochloric acid to obtain the high-surface-area porous carbon particles.
Example 4
As shown in fig. 1-3, in the pretreatment step, one or more of the mixture of the crushed pericarp, straw, leaves and fermentation residue agricultural and forestry waste is carbonized for 3 hours at 400 ℃ under nitrogen atmosphere, and then the mixture of ethanol and potassium hydroxide is mixed with the activated carbon according to a certain proportion and is pretreated in an oven at 80 ℃.
In the step of combining high-temperature pyrolysis, the pretreated sample is placed in nitrogen, and is heated to 400 ℃ to be activated for 3 hours, and then is heated to 800 ℃ to be carbonized for 3 hours.
And washing the carbonized sample by pure water, removing residual inorganic salt by hydrochloric acid, washing the sample to be neutral by pure water, and drying the sample in vacuum at 80 ℃ to obtain the final porous carbon particles with high specific surface area.
In the pretreatment step, one or more of crushed pericarp, straw, leaves and fermentation residue agricultural and forestry waste is/are placed in a nitrogen atmosphere to obtain plant activated carbon, then potassium hydroxide and 2g of activated carbon are mixed according to a mass ratio of 4:1 respectively, 60 ml of ethanol water solution with a volume ratio of 70% is added respectively, and after ultrasonic treatment is carried out for 30 minutes, the mixture is placed in an oven to be dried at 80 ℃.
In the high-temperature pyrolysis combined step, a sample is placed in nitrogen, heated to 400 ℃ at the speed of 5 ℃/min and activated for 3 hours, and then heated to 800 ℃ at the speed of 5 ℃/min for carbonization for 3 hours.
And centrifugally washing the carbonized sample to be neutral by pure water, adding 100 ml of hydrochloric acid solution with the concentration of 1 mol per liter, ultrasonically washing for 30 minutes, centrifugally washing to be neutral by water, and drying in a vacuum drying oven at 80 ℃ for 12 hours to obtain the final porous carbon particles with high specific surface area.
As shown in fig. 4 to 8, as a specific embodiment of the present invention, the oven used in the pretreatment step includes a box body 1, a feeding box 2; a discharge port 11 is formed in one side of the box body 1, and a conveying belt 3 and a heating resistance wire 4 are arranged in the box body 1; one movable end of the conveyor belt 3 is hinged to the discharge port 11, the other end of the conveyor belt 3 is hinged to the inner side wall of the box body 1, a heating resistance wire 4 is arranged above the conveyor belt 3, the heating resistance wire 4 is connected to the inner top surface of the box body 1, and the heating resistance wire 4 is used for drying materials; the outer side wall of the inner lower half part of the feeding box 2 is provided with a motor 21; an output shaft of the motor 21 extends into the feeding box 2, a roller 22 is arranged on the output shaft, and an extrusion block 221 is arranged on the surface of the roller 22; a discharge chute 23 is arranged on one side of the lower half part of the feeding box 2, an entity is arranged on one side of the discharge chute 23, a groove 24 is formed in the upper end of the entity, an extrusion block 221 is arranged on the inner surface of the groove 24, and a cavity is arranged on one side of the entity; the end part of the output shaft of the motor 21 is provided with a belt 211, the belt 211 is positioned in the cavity, and the end part of the output shaft of the motor 21 is connected with the other end of the conveyor belt 3 through the belt 211; mixing ethanol and potassium hydroxide with activated carbon according to a certain proportion, then putting the mixture into an oven for baking intervention treatment, pouring the material into a feeding box 2, enabling the material to flow into a groove 24 along the feeding box 2, driving a roller 22 to rotate by a motor 21 at the moment, enabling an extrusion block 221 on the surface of the roller 22 to be mutually meshed with an extrusion block 221 in the groove 24, grinding the material, further crushing the activated carbon, further mixing the ethanol and the potassium hydroxide with the activated carbon, improving the mixing degree of the material, then taking the material out of the groove 24 by the roller 22, and enabling the material to flow onto a conveyor belt 3 along a discharge groove 23; when motor 21 rotates, motor 21's output shaft passes through the electronic conveyer belt 3 operation of belt 211, and material flows to on the conveyer belt 3, then carries out drying process through the heat that heating resistor silk 4 produced, discharges from the discharge gate 11 department of box 1 at last, and this process is drying before the processing to the material, and the material rolls the thin fragmentation once more, improves the mixed degree between the material simultaneously, improves the effect of material preliminary treatment.
As a specific embodiment of the present invention, the surface of the conveyor belt 3 is uniformly provided with a plurality of rows of protrusions 31; the inner side of the discharge hole 11 is provided with a swing rod 111; one end of the swing rod 111 is hinged to the inner wall of the box body 1, the middle position of the swing rod 111 is connected to the inner side wall of the box body 1 through a spring 112 arranged on the inner wall of the box body 1, and the other end of the swing rod 111 is positioned between two adjacent rows of bulges 31 on the conveyor belt 3; the materials fall onto the conveyor belt 3, and the exposed surface area of the materials on the conveyor belt 3 is increased by the protrusions 31 on the conveyor belt 3, so that the drying amount of the heat to the materials on the conveyor belt 3 in unit area is increased, and the material drying intervention treatment efficiency is improved; the material is being about to move discharge gate 11 department, and protruding 31 bumps with the pendulum rod 111 is indirect, and protruding 31 extrudees pendulum rod 111, and pendulum rod 111 rotates around its pin joint, fails when contacting with protruding 31 at the other end of pendulum rod 111, and pendulum rod 111 is under the effect of spring 112, and the other end of pendulum rod 111 bumps with protruding 31, shakes the material on the conveyer belt 3 loose for the material breaks away from the conveyer belt 3 surface, avoids the adhesion of material on conveyer belt 3.
As a specific embodiment of the present invention, the heating resistance wire 4 is fixedly connected to a connection plate 411 arranged in the box body 1; one end of the connecting plate 411 is hinged to the inner top surface of the box body 1, and the other end of the connecting plate 411 is provided with a push rod 411; arc-shaped holes 12 symmetrically formed in the side wall of the box body 1 are penetrated through by the push rod 411, a limiting rod 412 is arranged on the part, located outside the box body 1, of the push rod 411, and two ends of the limiting rod 412 are embedded into fixing holes 121 formed in two sides of the arc-shaped holes 12; the push rod 411 moves up and down in the arc-shaped hole 12, the distance between the heating resistance wire 4 and the conveyor belt 3 is adjusted, the drying temperature of the heating resistance wire 4 to materials is controlled, and the phenomenon that the materials cannot meet the expected humidity when the materials are subjected to drying pretreatment is avoided.
The working principle is as follows: the materials are poured into the feeding box 2 and flow into the groove 24 along the feeding box 2, the motor 21 drives the roller 22 to rotate at the moment, the extrusion block 221 on the surface of the roller 22 is meshed with the extrusion block 221 in the groove 24, the materials are rolled, the activated carbon is further crushed, simultaneously, the ethanol and the potassium hydroxide are further mixed with the activated carbon, the mixing degree of the materials is improved, then the materials are taken out of the groove 24 by the roller 22, and the materials flow onto the conveyor belt 3 along the discharge chute 23; when motor 21 rotates, motor 21's output shaft passes through the electronic conveyer belt 3 operation of belt 211, and material flows to on the conveyer belt 3, then carries out drying process through the heat that heating resistor silk 4 produced, discharges from the discharge gate 11 department of box 1 at last, and this process is drying before the processing to the material, and the material rolls the thin fragmentation once more, improves the mixed degree between the material simultaneously, improves the effect of material preliminary treatment.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make several modifications and finishes without departing from the principle of the present invention, especially by using other alkali or salt containing potassium or sodium and ethanol together to pretreat the activated carbon sample, and these modifications and finishes should be considered as the protection scope of the present invention.
Claims (10)
1. A preparation method for producing layered porous activated carbon with high specific surface area is characterized in that: the preparation method comprises the following steps of firstly pretreating the activated carbon derived from agricultural and forestry waste (such as materials of fruit peels, straws, leaves or fermentation residues) at 70-100 ℃ by using ethanol and potassium hydroxide (the mass ratio is 1: 1-1: 6), and then carrying out high-temperature pyrolysis combination under the atmosphere of protective gas such as nitrogen and argon to finally obtain the high-surface-area porous carbon particles.
2. The preparation method for producing the layered porous activated carbon with high specific surface area according to claim 1, wherein: in the pretreatment step, one or more of the mixture of crushed pericarp, straw, leaves and fermentation residue agricultural and forestry waste is carbonized for 1-5 hours at 600 ℃ under nitrogen atmosphere at 300-.
3. The preparation method for producing the layered porous activated carbon with high specific surface area according to claim 2, wherein: in the pretreatment step, one or more of crushed pericarp, straw, leaves and fermentation residue agricultural and forestry waste is carbonized at 600 ℃ for 1-5 hours under nitrogen atmosphere to obtain plant activated carbon, then potassium hydroxide and 2g of activated carbon are mixed according to the mass ratio of 1:1, 2:1, 3:1, 4:1, 5:1 and 6:1 respectively, 50-100 ml of ethanol water solution with the volume ratio of 50%, 60%, 70%, 80% and 90% is added respectively, and after ultrasonic treatment is carried out for 30 minutes, the mixture is placed in an oven to be dried at 70-100 ℃.
4. The preparation method for producing the layered porous activated carbon with high specific surface area according to claim 1, wherein: in the step of combining the high-temperature pyrolysis, the pretreated sample is placed in nitrogen, and is heated to 500 ℃ for activation for 1-4 hours, and then is heated to 1000 ℃ for carbonization for 1-5 hours.
5. The preparation method for producing the layered porous activated carbon with high specific surface area according to claim 4, wherein: in the high-temperature pyrolysis combination step, the sample is put in nitrogen gas, heated to 500 ℃ at the speed of 5 ℃/min and activated for 1-4 hours, and then heated to 1000 ℃ at the speed of 5 ℃/min and carbonized for 1-5 hours.
6. The preparation method for producing the layered porous activated carbon with high specific surface area according to claim 5, wherein: and washing the carbonized sample by pure water, removing residual inorganic salt by hydrochloric acid, washing the sample to be neutral by pure water, and drying the sample in vacuum at 80 ℃ to obtain the final porous carbon particles with high specific surface area.
7. The preparation method for producing the layered porous activated carbon with high specific surface area according to claim 6, wherein: and centrifugally washing the carbonized sample to be neutral by pure water, adding 50-100 ml of hydrochloric acid solution with the concentration of 1 mol per liter, ultrasonically washing for 30 minutes, centrifugally washing to be neutral by water, and drying in a vacuum drying oven at 80 ℃ for 12 hours to obtain the final porous carbon particles with high specific surface area.
8. An oven for a manufacturing method of producing a layered porous activated carbon with a high specific surface area according to any one of claims 1 to 7, characterized in that: the oven used in the pretreatment step comprises a box body and a feeding box; a discharge port is formed in one side of the box body, and a conveying belt and a heating resistance wire are arranged in the box body; one end of the conveying belt is hinged at the discharge port, the other end of the conveying belt is hinged on the inner side wall of the box body, a heating resistance wire is arranged above the conveying belt and connected to the inner top surface of the box body, and the heating resistance wire is used for drying materials; a motor is arranged on the outer side wall of the lower half part in the feeding box; an output shaft of the motor extends into the feeding box, a roller is arranged on the output shaft, and an extrusion block is arranged on the surface of the roller; a discharge chute is arranged on one side of the lower half part of the feeding box, an entity is arranged on one side of the discharge chute, a groove is formed in the upper end of the entity, an extrusion block is arranged on the inner surface of the groove, and a cavity is arranged on one side of the entity; the end part of an output shaft of the motor is provided with a belt which is positioned in the cavity, and the end part of the output shaft of the motor is connected with the other end of the conveyor belt through the belt.
9. The preparation method for producing the layered porous activated carbon with high specific surface area according to claim 8, wherein: a plurality of rows of bulges are uniformly arranged on the surface of the conveyor belt; a swing rod is arranged on the inner side of the discharge hole; one end of the swing rod is hinged to the inner wall of the box body, the middle position of the swing rod is connected to the inner side wall of the box body through a spring arranged on the inner wall of the box body, and the other end of the swing rod is located between two adjacent rows of bulges on the conveying belt.
10. The preparation method for producing the layered porous activated carbon with high specific surface area according to claim 8, wherein: the heating resistance wire is fixedly connected to a connecting plate arranged in the box body; one end of the connecting plate is hinged to the inner top surface of the box body, and the other end of the connecting plate is provided with a push rod; the push rod runs through the arc-shaped holes symmetrically formed in the side wall of the box body, the part, located outside the box body, of the push rod is provided with a limiting rod, and two ends of the limiting rod are embedded into the fixing holes formed in two sides of the arc-shaped holes.
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