CN116553546A - Preparation method of biomass-based activated carbon with enhanced narrow pore distribution and stable similarity - Google Patents
Preparation method of biomass-based activated carbon with enhanced narrow pore distribution and stable similarity Download PDFInfo
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- CN116553546A CN116553546A CN202310606206.8A CN202310606206A CN116553546A CN 116553546 A CN116553546 A CN 116553546A CN 202310606206 A CN202310606206 A CN 202310606206A CN 116553546 A CN116553546 A CN 116553546A
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- pore distribution
- koh
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000011148 porous material Substances 0.000 title claims abstract description 56
- 239000002028 Biomass Substances 0.000 title claims abstract description 47
- 238000009826 distribution Methods 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 8
- 239000007790 solid phase Substances 0.000 claims abstract description 8
- 230000003213 activating effect Effects 0.000 claims abstract description 5
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims description 35
- 235000011613 Pinus brutia Nutrition 0.000 claims description 35
- 241000018646 Pinus brutia Species 0.000 claims description 35
- 239000002023 wood Substances 0.000 claims description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 16
- 239000000428 dust Substances 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 239000002699 waste material Substances 0.000 claims description 3
- 230000004913 activation Effects 0.000 abstract description 16
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000001965 increasing effect Effects 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000547 structure data Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method of biomass-based activated carbon with enhanced narrow pore distribution and stable similarity, which comprises the following steps: washing biomass raw materials with water, drying and crushing; solid KOH is dissolved in biomass raw materials by adopting a solid-phase ball milling process; applying a spatially confining force to the mixture of KOH and biomass feedstock; activating a mixture of KOH with a spatially confined force and a biomass feedstock; and cooling, crushing, acid washing and water washing the activated product, and drying the product in an oven until the weight is constant, thus obtaining the biomass-based activated carbon with enhanced narrow pore distribution and stable similarity. Compared with the biomass-based activated carbon prepared by directly activating the traditional KOH, the method has the advantages of improving the specific surface area, enhancing the narrow pore distribution strength, reducing the activation temperature and maintaining the similarity of the narrow pore distribution. The method can produce the active carbon with specific pore structure, so as to expand the application range of the active carbon, and has simple operation, lower production cost and obvious economic benefit.
Description
Technical Field
The invention relates to a preparation method of biomass-based activated carbon with enhanced narrow-pore distribution and stable similarity, belonging to the field of activated carbon production.
Background
Despite the rapid development of modern science, porous carbon remains the most important material in modern scientific, engineering and technical applications. The preparation and application of the biomass-based activated carbon are important actions for promoting sustainable development, assisting carbon to reach peak and neutralizing carbon. It is generally known that the specific surface area is one of the most important parameters determining the performance of activated carbon, and in this context, various preparation strategies have been developed (template method, order H 3 PO 4 -CO 2 Activation, sequential hydrothermal-activation) to produce activated carbon with high specific surface area and pore structure specificity. However, the template and sequence activation procedure is complex and energy consuming. It is therefore an important goal to explore a simple and easy manufacturing procedure (i.e., by-pass the template and sequential activation strategies) to obtain activated carbon with high specific surface area and specific pore structure (e.g., pore size distribution).
In addition to specific surface area, pore size distribution is also important for various applications of activated carbon. For example, the pore structure of the adsorbent should take into account the molecular size of the adsorbed material. The active carbon with abundant micropores, enough mesopores and a proper amount of macroporous structure is very ideal as an electrode material. Therefore, the increase of the micropore content on the basis of enough mesopores and a proper amount of macropores is beneficial to the improvement of the performance of the activated carbon electrode within a certain range. It is well known that increasing the level of activation (higher activator levels or temperatures) over a range can suitably increase the specific surface area, but the pore size or pore size distribution will likewise change. However, at a higher specific surface area [ ]>1000m 2 Again increasing the level of activation on the basis of/g) may result in the micropores collapsing into mesopores/macropores (i.e. the pore size distribution changes) with concomitant decrease in specific surface area. That is, at higher specific surface areas,the enhancement of the distribution intensity of narrow pores (e.g. 0-2 nm) encounters a bottleneck. In addition, KOH is widely used as an ideal activator for producing activated carbon having a high specific surface area.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of biomass-based activated carbon with enhanced narrow pore distribution and stable similarity, which aims at overcoming the defects of the prior art, and the preparation method has the advantages of enhancing the narrow pore distribution strength, reducing energy consumption, improving the specific surface area, expanding the application range, improving the quality of the carbon and achieving the multi-win effects of economic benefit, high value and the like on the basis of maintaining the similar pore size distribution.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the preparation method of the biomass-based activated carbon with enhanced narrow pore distribution and stable similarity comprises the following steps:
(1) Washing the biomass raw material with water, drying and crushing;
(2) Solid KOH is dissolved in biomass raw materials by adopting a solid-phase ball milling process;
(3) Applying a spatially confining force to the mixture of KOH and biomass feedstock;
(4) Activating a mixture of KOH with a spatial domain limiting force and a biomass raw material;
(5) And cooling, crushing, acid washing and water washing the activated product, and drying the product in an oven until the weight is constant.
As a further improved technical scheme of the invention, the biomass raw material is pine wood dust, pine needles or artificial board waste.
As a further improved technical scheme of the invention, in the step (1), the biomass raw material is washed with water, dried and crushed to 20-40 meshes.
As a further improved technical scheme of the invention, in the step (2), the mass ratio of the solid KOH to the biomass raw material is 3:1, ball milling time is 20min.
As a further improved technical scheme of the invention, in the step (3), the mixture of KOH and biomass raw material is applied with space limiting force through a tablet press.
As a further improved technical scheme of the invention, in the step (3), the mixture of the solid KOH and the biomass raw material is extruded for 15min by the force of 10-40MPa applied by a tablet press in a die with the diameter of 1 cm.
As a further improved technical scheme of the invention, in the step (4), the mixture of KOH with space limiting force and biomass raw materials is placed in a nickel ark and activated for a certain time in a tube furnace.
As a further improved technical scheme of the invention, in the step (4), the temperature of the tube furnace is 750-850 ℃, and the heat preservation time is 60min.
As a further improved technical scheme of the invention, the temperature of the oven is 105 ℃.
The beneficial effects of the invention are as follows:
(1) The preparation method of the biomass-based activated carbon can maintain the similarity of pore size distribution, enhance the distribution strength of narrow pores and improve the specific surface area;
(2) The preparation method of the biomass-based activated carbon can reduce energy consumption, expand the application range of the carbon and improve the quality of the carbon, thereby achieving the multi-win effects of economic benefit, high value and the like.
Drawings
FIG. 1 is a flow diagram of a method for preparing biomass-based activated carbon with enhanced narrow pore distribution but stable similarity.
Fig. 2 (a) is a graph of nitrogen adsorption and desorption of activated carbon obtained by changing conventional activation conditions.
Fig. 2 (b) is a pore size distribution diagram of activated carbon obtained by changing conventional activation conditions.
Fig. 3 (a) is a graph showing the desorption of nitrogen from activated carbon obtained by changing the space-limiting force at an activation temperature of 750 ℃.
Fig. 3 (b) is a pore size distribution diagram of activated carbon obtained by changing the space-limiting force at an activation temperature of 750 ℃.
Fig. 4 (a) is a nitrogen adsorption and desorption curve of activated carbon obtained by changing the space-limiting force at an activation temperature of 850 ℃.
Fig. 4 (b) is a pore size distribution diagram of the activated carbon obtained by changing the space-limiting force at an activation temperature of 850 ℃.
Detailed Description
The invention will be further illustrated with reference to specific examples. The experimental methods in the following examples are conventional methods unless otherwise specified.
Raw materials: pine wood chips, KOH (analytically pure), hydrochloric acid.
The main device comprises: tablet press, die (diameter 1 cm), high temperature tube furnace, oven, autosorb-iQ full-automatic gas adsorption analyzer.
Example 1:
washing pine wood scraps with water, drying, crushing to 20-40 meshes, and adopting a solid-phase ball milling process to dissolve 12g of solid KOH into 4g of pine wood scraps. The mixture of pine wood chips and KOH was placed in a die having a diameter of 1cm, and then a pressure of 30MPa was applied by a tablet press and maintained for 15 minutes. Next, the mixture of KOH with space-limiting force and pine dust was placed in a nickel ark and activated in a tube furnace at 750 ℃ for 60min. Finally, the activated product is cooled, crushed, washed with acid, washed with water, and dried in an oven at 105 ℃ to constant weight, thus obtaining the pine-based activated carbon (named PC-30-750).
The traditional method comprises the following steps: mixing KOH solid and pine wood dust in a mass ratio of 3, and then placing the mixture into a nickel square boat and activating the mixture in a tube furnace at 750, 800 and 850 ℃ for 60min respectively; finally, cooling, crushing, acid washing and water washing the activated product, and drying the product in an oven at 105 ℃ to constant weight to obtain the pine-based activated carbon (named as PC-0-750, PC-0-800 and PC-0-850). The characteristics of PC-30-750 prepared in this example and PC-0-750, PC-0-800 and PC-0-850 prepared by the conventional method are shown in (a) in FIG. 2, (b) in FIG. 2, (a) in FIG. 3, (b) in FIG. 3 and Table 1.
Table 1 is sample well structure data:
as can be seen from fig. 2 (a), 2 (b) and table 1, changing the activation level (e.g., activation temperature) during the conventional process for preparing activated carbon increases the specific surface area in a certain range but also significantly changes the pore size distribution, exhibiting average pore diameters of 2.09nm (PC-0-750), 2.23nm (PC-0-800) and 2.05nm (PC-0-850), respectively. It is noted that, as can be seen from (a) in fig. 3, (b) in fig. 3 and table 1, the specific surface area of the pine-based activated carbon (PC-30-750) prepared under the space-limited force of 30MPa is significantly higher than that of PC-0-750 and slightly higher than that of PC-0-850, which indicates that the present implementation can significantly reduce the activation temperature (energy consumption). In addition, the narrow pore distribution intensity of PC-30-750 was significantly enhanced compared to PC-0-750, but the narrow pore distribution curves of both were highly similar, exhibiting average pore diameters of 2.09nm (PC-0-750) and 2.08nm (PC-30-750), respectively. It is apparent that the average pore size is considered to be consistent over the error range.
Example 2:
washing pine wood scraps with water, drying, crushing to 20-40 meshes, and adopting a solid-phase ball milling process to dissolve 12g of solid KOH into 4g of pine wood scraps. The mixture of pine wood chips and KOH was placed in a die having a diameter of 1cm, and then a pressure of 10MPa was applied by a tablet press and maintained for 15 minutes. Next, the mixture of KOH with space-limiting force and pine dust was placed in a nickel ark and activated in a tube furnace at 850 ℃ for 60min. Finally, cooling, crushing, acid washing and water washing the activated product, and drying the product in an oven at 105 ℃ to constant weight to obtain the pine-based activated carbon (named as PC-10-850). As can be seen from FIG. 4 (a), FIG. 4 (b) and Table 1, the specific surface area of PC-10-850 is increased relative to PC-0-850, and the narrow pore distribution intensity is enhanced, but the narrow pore distribution curves of the two samples remain similar. At the same time, the average pore diameters of the two samples can be considered to be consistent within the error range.
Example 3:
washing pine wood scraps with water, drying, crushing to 20-40 meshes, and adopting a solid-phase ball milling process to dissolve 12g of solid KOH into 4g of pine wood scraps. The mixture of pine wood chips and KOH was placed in a die having a diameter of 1cm, and then a pressure of 20MPa was applied by a tablet press and maintained for 15 minutes. Next, the mixture of KOH with space-limiting force and pine dust was placed in a nickel ark and activated in a tube furnace at 850 ℃ for 60min. Finally, cooling, crushing, acid washing and water washing the activated product, and drying the product in an oven at 105 ℃ to constant weight to obtain the pine-based activated carbon (named as PC-20-850). As can be seen from FIG. 4 (a), FIG. 4 (b) and Table 1, the specific surface area of PC-20-850 is increased relative to PC-0-850 and PC-10-850, and the narrow pore distribution intensity is enhanced, but the narrow pore distribution curves of the three samples remain similar. At the same time, the average pore diameters of the three samples can be considered to be consistent within the error range.
Example 4:
washing pine wood scraps with water, drying, crushing to 20-40 meshes, and adopting a solid-phase ball milling process to dissolve 12g of solid KOH into 4g of pine wood scraps. The mixture of pine wood chips and KOH was placed in a die having a diameter of 1cm, and then a pressure of 30MPa was applied by a tablet press and maintained for 15 minutes. Next, the mixture of KOH with space-limiting force and pine dust was placed in a nickel ark and activated in a tube furnace at 850 ℃ for 60min. Finally, cooling, crushing, acid washing and water washing the activated product, and drying the product in an oven at 105 ℃ to constant weight to obtain the pine-based activated carbon (named as PC-30-850). As can be seen from FIG. 4 (a), FIG. 4 (b) and Table 1, the specific surface area of PC-30-850 is increased and the narrow pore distribution intensity is enhanced with respect to PC-0-850, PC-10-850 and PC-20-850, but the narrow pore distribution curves of the four samples remain similar. At the same time, the average pore size of the four samples can be considered to be consistent within the error range.
Example 5:
washing pine wood scraps with water, drying, crushing to 20-40 meshes, and adopting a solid-phase ball milling process to dissolve 12g of solid KOH into 4g of pine wood scraps. The mixture of pine wood chips and KOH was placed in a die having a diameter of 1cm, and then a pressure of 40MPa was applied by a tablet press and maintained for 15 minutes. Next, the mixture of KOH with space-limiting force and pine dust was placed in a nickel ark and activated in a tube furnace at 850 ℃ for 60min. Finally, cooling, crushing, acid washing and water washing the activated product, and drying the product in an oven at 105 ℃ to constant weight to obtain the pine-based activated carbon (named as PC-40-850). As can be seen from FIG. 4 (a), FIG. 4 (b) and Table 1, the specific surface area of PC-40-850 increases and the narrow pore distribution intensity increases with respect to PC-0-850, PC-10-850, PC-20-850 and PC-30-850, but the narrow pore distribution curves of the five samples remain similar. At the same time, the average pore diameters of the five samples can be considered to be consistent within the error range.
In conclusion, in the invention, the specific surface area of the biomass-based activated carbon prepared under the action of the space-limited force of 10-40MPa is obviously higher than that of the activated carbon prepared under the action of the non-space-limited force, which shows that the preparation method can maintain the similarity of pore size distribution, enhance the narrow pore distribution intensity and improve the specific surface area; meanwhile, the activation temperature (energy consumption) can be obviously reduced, the application range of the carbon is expanded, and the quality of the carbon is improved, so that the multi-win effects of economic benefit, high value and the like are achieved.
The biomass raw materials, such as pine wood dust, can also be replaced by pine needles or artificial board waste.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to apply equivalents and modifications to the technical solution and the inventive concept thereof within the scope of the present invention.
Claims (9)
1. A method for preparing biomass-based activated carbon with enhanced narrow pore distribution and stable similarity, which is characterized by comprising the following steps:
(1) Washing the biomass raw material with water, drying and crushing;
(2) Solid KOH is dissolved in biomass raw materials by adopting a solid-phase ball milling process;
(3) Applying a spatially confining force to the mixture of KOH and biomass feedstock;
(4) Activating a mixture of KOH with a spatial domain limiting force and a biomass raw material;
(5) And cooling, crushing, acid washing and water washing the activated product, and drying the product in an oven until the weight is constant.
2. The method for preparing biomass-based activated carbon with enhanced narrow pore distribution and stable similarity according to claim 1, wherein the biomass raw material is pine wood dust, pine needles or artificial board waste.
3. The method for preparing biomass-based activated carbon with enhanced narrow pore distribution but stable similarity according to claim 1, wherein in the step (1), the biomass raw material is washed with water, dried and pulverized to 20-40 mesh.
4. The method for preparing biomass-based activated carbon with enhanced narrow pore distribution and stable similarity according to claim 1, wherein in the step (2), the mass ratio of solid KOH to biomass raw material is 3:1, ball milling time is 20min.
5. The method for preparing biomass-based activated carbon with enhanced narrow pore distribution but stable similarity according to claim 1, wherein in the step (3), a mixture of KOH and biomass raw material is subjected to a spatially-limited force by a tablet press.
6. The method for preparing a biomass-based activated carbon with enhanced narrow pore distribution but stable similarity according to claim 5, wherein in the step (3), the mixture of solid KOH and biomass raw material is pressed for 15min by a force of 10-40MPa applied by a tablet press in a die with a diameter of 1 cm.
7. The method for preparing a biomass-based activated carbon with enhanced narrow pore distribution but stable similarity according to claim 1, wherein in the step (4), a mixture of KOH with space-limiting force and biomass raw material is placed in a nickel square boat and activated in a tube furnace for a certain time.
8. The method for preparing biomass-based activated carbon with enhanced narrow pore distribution and stable similarity according to claim 7, wherein in the step (4), the tube furnace temperature is 750-850 ℃ and the holding time is 60min.
9. The method for preparing biomass-based activated carbon with enhanced narrow pore distribution but stable similarity according to claim 1, wherein the temperature of the oven is 105 ℃.
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