CN111530440A - Preparation method of coal-based porous material - Google Patents
Preparation method of coal-based porous material Download PDFInfo
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- CN111530440A CN111530440A CN202010378190.6A CN202010378190A CN111530440A CN 111530440 A CN111530440 A CN 111530440A CN 202010378190 A CN202010378190 A CN 202010378190A CN 111530440 A CN111530440 A CN 111530440A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
Abstract
The invention relates to the field of production and preparation of porous materials, in particular to a preparation method of a coal-based porous material. The preparation method of the coal-based porous material comprises the following steps: step S1: coal tar coke is used for preparing coal powder; step S2: using coal powder to prepare a carbon source; step S3: making the carbon source into porous carbon; step S4: activating the porous carbon. The embodiment of the invention has the beneficial effects that: the coal powder is made into the carbon source, then the carbon source is made into the porous carbon, and the porous carbon is activated to obtain the porous material with high activity and high adsorbability, so that the production cost of the porous material is reduced, and the adsorption efficiency of the porous material can be improved.
Description
Technical Field
The invention relates to the field of production and preparation of porous materials, in particular to a preparation method of a coal-based porous material.
Background
The existing porous materials for adsorption have more types, and how to improve the adsorption performance of the adsorption material at lower cost is a technical problem to be solved in the prior art.
Disclosure of Invention
The invention aims to provide a preparation method of a coal-based porous material, which can utilize coal base as a low cost and produce a high-adsorption porous material with good activity.
The embodiment of the invention is realized by the following steps:
a preparation method of a coal-based porous material comprises the following steps:
step S1: coal tar coke is used for preparing coal powder;
step S2: using coal powder to prepare a carbon source;
step S3: making the carbon source into porous carbon;
step S4: activating the porous carbon.
In a preferred embodiment of the present invention, the method for manufacturing the carbon source comprises:
placing the mixture of the coal powder and the 1-methylnaphthalene extractant in an extraction kettle, heating to 350 ℃, keeping the temperature at 350 ℃ for 1 hour to finish the extraction process, then cooling the kettle to room temperature, and separating the mixture to obtain the carbon source.
In the preferred embodiment of the present invention, the temperature increase rate in step S2 is 5 deg.C/min-15 deg.C/min.
In a preferred embodiment of the present invention, in step S3, the method for making the carbon source into porous carbon comprises:
magnesium oxide, the carbon source and dimethylformamide according to the mass ratio of 1:20:40, standing, drying, putting the mixed solution after stirring into a nitrogen environment, heating to 350-650 ℃, and keeping for 1 hour; continuously heating to 700-1000 ℃, keeping for 3 hours, and finishing carbonization.
In a preferred embodiment of the invention, the product after the activation is washed with acid to remove magnesium oxide, then washed with water to remove magnesium ions and chloride ions, and finally dried to obtain the porous carbon to be activated.
In a preferred embodiment of the present invention, in step S4, the method for activating the porous carbon comprises:
and (3) mixing potassium hydroxide, absolute ethyl alcohol, deionized water and the porous carbon obtained in the step S3 in a mass ratio of 4:5: 10: 1, stirring, drying at 800 deg.C and N2Environment(s)Activating for 3 hours to obtain activated porous carbon.
In the preferred embodiment of the invention, the activated porous carbon is washed by water and acid to be neutral, and then dried to obtain the high-activity adsorption porous material.
In the preferred embodiment of the present invention, hydrochloric acid is used in an amount of L mol/L.
In a preferred embodiment of the present invention, the method for manufacturing the carbon source comprises:
drying, crushing and grinding raw coal, adding an adhesive to uniformly knead the adhesive and coal powder, layering, molding and drying.
In the preferred embodiment of the invention, the activated porous carbon is treated at 2800 ℃ to obtain graphitized foam carbon.
The embodiment of the invention has the beneficial effects that:
the coal powder is made into the carbon source, then the carbon source is made into the porous carbon, and the porous carbon is activated to obtain the porous material with high activity and high adsorbability, so that the production cost of the porous material is reduced, and the adsorption efficiency of the porous material can be improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a flow chart of a method for preparing a coal-based porous material according to an embodiment of the present invention;
fig. 2 is a flowchart of a method for manufacturing a carbon source in a method for manufacturing a coal-based porous material according to an embodiment of the present invention;
fig. 3 is a flowchart of a method for manufacturing a carbon source into porous carbon in a preparation method of a coal-based porous material according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, 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 some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. 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.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are conventionally placed in use, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal", "vertical", "overhang" and the like do not imply that the components are required to be absolutely horizontal or overhang, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Some embodiments of the invention are described in detail below with reference to figures 1-3. The embodiments described below and the features of the embodiments can be combined with each other without conflict.
A preparation method of a coal-based porous material, as shown in fig. 1, comprising the following steps:
step S1: coal tar coke is used for preparing coal powder;
step S2: using coal powder to prepare a carbon source;
step S3: making the carbon source into porous carbon;
step S4: activating the porous carbon.
Specifically, in this embodiment, coal powder is used as a raw material, the coal powder is firstly made into a carbon source of porous carbon, the carbon source is then made into the porous carbon, and finally, the porous carbon is activated to obtain the final coal-based porous material with a high adsorption effect.
The preparation process of the coal dust in the embodiment is as follows:
freezing and embrittling the high-temperature coal tar pitch coke at low temperature, adding a surfactant, crushing the coal tar pitch coke by using a high-speed crusher, and screening to obtain coal tar pitch powder with the granularity of less than or equal to 200 meshes and capable of being stably stored at room temperature.
In the embodiment, the coal powder is prepared by using the low-temperature brittleness of materials and adopting a freezing and crushing technology, but the coal pitch coke powder with the granularity of less than or equal to 200 meshes has larger surface energy and is easy to agglomerate, so that a surfactant needs to be added in the preparation process.
Specifically, the medium-temperature coal tar pitch coke fragments with the softening point of 90 ℃ are respectively preserved for 24 hours at 15 ℃ and 25 ℃ below zero, crushed for 30s and sieved by a standard sieve of 200 meshes. When the storage temperatures of the raw materials are respectively 15 ℃ and-25 ℃, the crushing effects are not greatly different (the screen residue rates are respectively 24.77 percent and 23.87 percent), which indicates that the embrittlement temperature of the coal tar pitch coke is below 15 ℃.
Crushing the medium-temperature coal tar pitch coke fragments stored at 15 ℃ and-25 ℃ for 30s to obtain coal tar pitch coke powder with good dispersibility; if the crushing process is continued for 30 seconds, the asphalt coke powder becomes a block solid with certain viscosity because the heat is generated to agglomerate the asphalt coke powder when the crushing process is carried out for a long time. Therefore, the crushing time is controlled to be 30s, and the crushing temperature can be reduced by an external cold source if necessary.
In a preferred embodiment of the present invention, as shown in fig. 2, the method for manufacturing the carbon source comprises:
placing the mixture of the coal powder and the 1-methylnaphthalene extractant in an extraction kettle, heating to 350 ℃, keeping the temperature at 350 ℃ for 1 hour to finish the extraction process, then cooling the kettle to room temperature, and separating the mixture to obtain the carbon source.
Specifically, in this example, a mixture of 250 μm to 841 μm coal dust and 1-methylnaphthalene extractant was placed in a self-made batch extractor, the temperature was programmed to 350 ℃, and maintained at 350 ℃ for 1 hour, thereby completing the extraction process.
Then, after the pot temperature was decreased to room temperature, the mixture was separated.
Finally, the yield of the extract was 32.33 wt% (dry ashless basis, daf), and the extract was used as a carbon source for preparing porous carbon.
During the whole manufacturing process, the sealing property in the extraction kettle needs to be maintained.
In the preferred embodiment of the present invention, the temperature increase rate in step S2 is 5 deg.C/min-15 deg.C/min.
Specifically, when the temperature is raised in the extraction kettle, the extraction effect is affected by the too fast or too slow temperature raising rate, and in order to ensure the extraction effect, the temperature raising rate selected in this embodiment is 5 ℃/min to 15 ℃/min, wherein, preferably, the temperature raising rate is 5 ℃/min.
In a preferred embodiment of the present invention, in step S3, as shown in fig. 3, the method for making the carbon source into porous carbon comprises:
magnesium oxide, the carbon source and dimethylformamide according to the mass ratio of 1:20:40, standing, drying, putting the mixed solution after stirring into a nitrogen environment, heating to 350-650 ℃, and keeping for 1 hour; continuously heating to 700-1000 ℃, keeping for 3 hours, and finishing carbonization.
Specifically, adding magnesium oxide, an extracted carbon source and Dimethylformamide (DMF) into a beaker according to the mass ratio of 1:20:40, stirring, standing overnight, and then placing the mixed solution after standing overnight into a 120 ℃ forced air drying oven for drying: then placing the mixture into a tubular furnace in nitrogen atmosphere, heating to 350 ℃, and keeping for 1 h; the temperature is continuously increased to 800 ℃ and kept for 3 hours, and the temperature rising rate is 5 ℃/min.
In a preferred embodiment of the invention, the product after the activation is washed with acid to remove magnesium oxide, then washed with water to remove magnesium ions and chloride ions, and finally dried to obtain the porous carbon to be activated.
The carbonized product is repeatedly soaked by 3mol/L hydrochloric acid to remove magnesium oxide, and then is washed by a large amount of deionized water to remove magnesium ions and chloride ions. Finally, the product was dried by air blowing at 120 ℃ for 8 hours to obtain "porous carbon before activation" in a yield of 44.96 wt% (daf) with respect to the extract.
In a preferred embodiment of the present invention, in step S4, the method for activating the porous carbon comprises:
and (3) mixing potassium hydroxide, absolute ethyl alcohol, deionized water and the porous carbon obtained in the step S3 in a mass ratio of 4:5: 10: 1, stirring, drying at 800 deg.C and N2Activating for 3 hours under the environment to obtain activated porous carbon.
In order to further enrich the pore structure of the material and improve the specific surface area of the material, the porous carbon before activation is subjected to potassium hydroxide activation treatment. Porous carbon before activation, potassium hydroxide, absolute ethyl alcohol and deionized waterAdding the mixture into a beaker according to the mass ratio of 1:4:5:10, stirring the mixture overnight, and blowing and drying the mixture at 120 ℃. Then, the mixture was heated at 800 ℃ N2And (3) activating in a tubular furnace for 3 hours under the atmosphere, wherein the heating rate is 5 ℃/min.
In the preferred embodiment of the invention, the activated porous carbon is washed by water and acid to be neutral, and then dried to obtain the high-activity adsorption porous material.
The activated mixture was neutralized by washing with water and acid, and dried by blowing at 120 ℃ for 8 hours to obtain "activated porous carbon" having a yield of 53.38 wt% fdaf with respect to the porous carbon before activation).
In the preferred embodiment of the present invention, hydrochloric acid is used in an amount of L mol/L.
In the present embodiment, hydrochloric acid may be used as the acid washing, and sulfuric acid, carbonic acid, or the like may be used as long as the porous carbon can be neutralized.
Specifically, in this embodiment, deionized water is used during the water washing, so that magnesium ions and chloride ions can be effectively removed.
In a preferred embodiment of the present invention, the method for manufacturing the carbon source comprises:
drying, crushing and grinding raw coal, adding an adhesive to uniformly knead the adhesive and coal powder, layering, molding and drying.
Drying, crushing and grinding raw coal, mixing the raw coal and the ground coal according to a certain proportion, adding a certain adhesive (40g/100g coal), uniformly kneading the mixture and coal powder in a kneader, and pressing the mixture into strips in a strip extruder; after the sample is dried, the material strip is carbonized in an external heating carbonization furnace, the carbonization temperature is increased to 650 ℃ from room temperature at the speed of 12 ℃/min, and the sample tube is taken out and naturally cooled; 400g of the carbonized material is placed in an activation tube, water is supplied at a rate of 5mL/min when the temperature rises to 650 ℃, and the activation time is recorded when the temperature rises to 940 ℃.
Specifically, in this embodiment, the binder is coal tar pitch.
In the preferred embodiment of the invention, the activated porous carbon is treated at 2800 ℃ to obtain graphitized foam carbon.
The obtained carbon foam is graphitized at 2800 ℃ when the foaming temperature is 500 ℃ and the foaming pressure is 3 MPa.
Therefore, the method for producing the carbon source by using the pulverized coal has multiple modes, and the activation mode of the porous carbon also has multiple modes, so that the porous carbon can be used as an adsorption material for producing the porous material with the pulverized coal, the method is convenient, the cost is low, the adsorption efficiency is ensured, and the manufacturing cost is reduced.
The embodiment of the invention has the beneficial effects that:
the coal powder is made into the carbon source, then the carbon source is made into the porous carbon, and the porous carbon is activated to obtain the porous material with high activity and high adsorbability, so that the production cost of the porous material is reduced, and the adsorption efficiency of the porous material can be improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the coal-based porous material is characterized by comprising the following steps:
step S1: coal tar coke is used for preparing coal powder;
step S2: using coal powder to prepare a carbon source;
step S3: making the carbon source into porous carbon;
step S4: activating the porous carbon.
2. The preparation method of the coal-based porous material according to claim 1, wherein the method for preparing the charcoal source comprises the following steps:
placing the mixture of the coal powder and the 1-methylnaphthalene extractant in an extraction kettle, heating to 350 ℃, keeping the temperature at 350 ℃ for 1 hour to finish the extraction process, then cooling the kettle to room temperature, and separating the mixture to obtain the carbon source.
3. The method for preparing a coal-based porous material according to claim 2, wherein the temperature increase rate in step S2 is 5 ℃/min to 15 ℃/min.
4. The method for preparing the coal-based porous material according to claim 1, wherein in step S3, the method for preparing the carbon source into the porous carbon comprises:
magnesium oxide, the carbon source and dimethylformamide according to the mass ratio of 1:20:40, standing, drying, putting the mixed solution after stirring into a nitrogen environment, heating to 350-650 ℃, and keeping for 1 hour; continuously heating to 700-1000 ℃, keeping for 3 hours, and finishing carbonization.
5. The preparation method of the coal-based porous material as claimed in claim 4, wherein the carbonized product is subjected to acid washing to remove magnesium oxide, then is subjected to water washing to remove magnesium ions and chloride ions, and finally, is dried to obtain the porous carbon to be activated.
6. The method for preparing the coal-based porous material according to claim 1, wherein in step S4, the method for activating the porous carbon is as follows:
and (3) mixing potassium hydroxide, absolute ethyl alcohol, deionized water and the porous carbon obtained in the step S3 in a mass ratio of 4:5: 10: 1, stirring, drying at 800 deg.C and N2Activating for 3 hours under the environment to obtain activated porous carbon.
7. The preparation method of the coal-based porous material as claimed in claim 6, wherein the activated porous carbon is washed with water and acid to neutrality, and then dried to obtain the high-activity adsorption porous material.
8. The method for preparing the coal-based porous material according to claim 7, wherein lmol/L hydrochloric acid is used for acid washing.
9. The preparation method of the coal-based porous material according to claim 1, wherein the method for preparing the charcoal source comprises the following steps:
drying, crushing and grinding raw coal, adding an adhesive to uniformly knead the adhesive and coal powder, layering, molding and drying.
10. The method for preparing the coal-based porous material according to claim 1, wherein the activated porous carbon is treated at a high temperature of 2800 ℃ to obtain graphitized foam carbon.
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