CN116495733B - Preparation method of bamboo activated carbon with high specific surface area and bamboo activated carbon - Google Patents
Preparation method of bamboo activated carbon with high specific surface area and bamboo activated carbon Download PDFInfo
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- CN116495733B CN116495733B CN202310736218.2A CN202310736218A CN116495733B CN 116495733 B CN116495733 B CN 116495733B CN 202310736218 A CN202310736218 A CN 202310736218A CN 116495733 B CN116495733 B CN 116495733B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 182
- 235000017166 Bambusa arundinacea Nutrition 0.000 title claims abstract description 69
- 235000017491 Bambusa tulda Nutrition 0.000 title claims abstract description 69
- 241001330002 Bambuseae Species 0.000 title claims abstract description 69
- 235000015334 Phyllostachys viridis Nutrition 0.000 title claims abstract description 69
- 239000011425 bamboo Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 130
- 239000000843 powder Substances 0.000 claims abstract description 77
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000002002 slurry Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000011269 tar Substances 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 238000010000 carbonizing Methods 0.000 claims abstract description 14
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 230000003213 activating effect Effects 0.000 claims abstract description 5
- 238000001994 activation Methods 0.000 claims description 23
- 230000004913 activation Effects 0.000 claims description 21
- 239000002244 precipitate Substances 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000003763 carbonization Methods 0.000 claims description 7
- 238000004898 kneading Methods 0.000 claims description 7
- 239000000835 fiber Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 3
- 241000264877 Hippospongia communis Species 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 9
- 230000008569 process Effects 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000010440 gypsum Substances 0.000 description 14
- 229910052602 gypsum Inorganic materials 0.000 description 14
- 239000011148 porous material Substances 0.000 description 13
- 238000006477 desulfuration reaction Methods 0.000 description 12
- 230000023556 desulfurization Effects 0.000 description 12
- 239000006227 byproduct Substances 0.000 description 10
- 230000006872 improvement Effects 0.000 description 8
- 239000012299 nitrogen atmosphere Substances 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- 235000013162 Cocos nucifera Nutrition 0.000 description 2
- 244000060011 Cocos nucifera Species 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003546 flue gas Substances 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000006028 limestone Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- JGIATAMCQXIDNZ-UHFFFAOYSA-N calcium sulfide Chemical compound [Ca]=S JGIATAMCQXIDNZ-UHFFFAOYSA-N 0.000 description 1
- 239000005539 carbonized material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 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
- C01B32/336—Preparation characterised by gaseous activating agents
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the technical field of activated carbon, and discloses a preparation method of high-specific-surface-area bamboo activated carbon and the bamboo activated carbon. The preparation method of the bamboo activated carbon with the high specific surface area comprises the following steps: (1) Carbonizing a powder body comprising fresh bamboo powder to obtain carbon powder; (2) Extruding and molding slurry comprising carbon powder, tar and water to obtain a blank; (3) carbonizing the blank to obtain a precursor; (4) Activating the precursor to obtain the bamboo activated carbon with high specific surface area; wherein the powder and/or slurry further comprises calcium sulfate powder. The method has the advantages of simple and easily controlled process, high production efficiency, green and environment-friendly raw materials, low cost, high specific surface area, good adsorption performance, long service life and extremely strong practicability, and can be implemented by directly adopting equipment of the traditional process.
Description
Technical Field
The invention relates to the technical field of activated carbon, in particular to a preparation method of high-specific-surface-area bamboo activated carbon and the bamboo activated carbon.
Background
The activated carbon has special microcrystalline structure, developed pores, large specific surface area, double physical adsorption and chemical adsorption characteristics, and can selectively adsorb various substances in liquid phase and gas phase, so that the activated carbon is often used as an excellent adsorbent to achieve the purposes of decolorization refining, disinfection deodorization, decontamination purification and the like, and is widely applied to the fields of foods, beverages, medicines, water treatment, gas purification and recovery, chemical industry, smelting, agriculture and the like. In recent years, with the increasing demands of people on living environments such as safety, purity and the like, the market demands of activated carbon are expanding, and the demands on adsorptivity, controllability, safety and the like of the activated carbon are increasing. Therefore, biomass activated carbon, especially bamboo activated carbon, is widely studied because of abundant raw materials and environment friendliness and easy acquisition, and developed microporous activated carbon is also an important point for development because of better adsorption performance.
In general, the higher the specific surface area of activated carbon, the better the adsorption performance. The preparation process of the bamboo activated carbon mainly comprises the steps of proportioning, kneading, extrusion molding, carbonization and activation, wherein the influence of the activation process on the pore structure and the specific surface area of the activated carbon is most remarkable. Currently, the activation methods mainly include a physical activation method and a chemical activation method. The chemical activation method mainly mixes carbonized material with activating agents such as zinc chloride, phosphoric acid, nitric acid and the like and carries out heat treatment, and the heat treatment temperature is different according to the different activating agents. The chemical activation method introduces new chemical reagent, which is large in dosage and generally not friendly to equipment and environment, and further requires complex recovery procedures, which is not beneficial to the safe use of the activated carbon. The physical activation method mainly uses water vapor, carbon dioxide or a mixed gas of the water vapor and the carbon dioxide as an activation atmosphere, and carries out oxidation reaction of carbon at high temperature to prepare the active carbon with a vigorous pore structure. The physical activation method does not adopt chemical reagent, is more environment-friendly and is a commonly used activation method at present.
Currently, the mainstream biomass activated carbon with high specific surface area is coconut activated carbon, but the coconut raw material is limited and the production cost is high. The bamboo activated carbon has rich raw materials and low production cost, but the specific surface area of the bamboo activated carbon prepared by the traditional process is generally below 1000 square meters per gram, and the bamboo activated carbon with high specific surface area is difficult to prepare.
Disclosure of Invention
The invention mainly aims to provide a preparation method of bamboo activated carbon with high specific surface area and the bamboo activated carbon, so as to solve the technical problem of low specific surface area of the bamboo activated carbon in the prior art.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a method for preparing a high specific surface area bamboo activated carbon, comprising the steps of:
the preparation method of the bamboo activated carbon with the high specific surface area comprises the following steps:
(1) Carbonizing a powder body comprising fresh bamboo powder to obtain carbon powder;
(2) Extruding and molding slurry comprising carbon powder, tar and water to obtain a blank;
(3) Carbonizing the blank to obtain a precursor;
(4) Activating the precursor to obtain the bamboo activated carbon with high specific surface area;
wherein the powder and/or slurry further comprises calcium sulfate powder.
As a further improvement of the first aspect of the invention: the calcium sulfate powder is calcium sulfate whisker powder; and/or the calcium sulfate powder is desulfurization byproduct gypsum.
As a further improvement of the first aspect of the invention: the calcium sulfate whisker is mainly composed of fibers with the length of 100-460 mu m and the width of 12-25 mu m.
As a further improvement of the first aspect of the invention: the preparation of the calcium sulfate whisker comprises the following steps: adding sulfuric acid into the calcium oxide aqueous dispersion, and then collecting, washing and drying the generated precipitate; dispersing the precipitate in sulfuric acid, heating, standing at room temperature until the precipitate is separated out after the precipitate is completely dissolved, and collecting, washing and drying the separated precipitate to obtain the calcium sulfate whisker.
As a further improvement of the first aspect of the invention: when the powder contains calcium sulfate powder, the weight of the calcium sulfate powder is 10-15% of that of the fresh bamboo powder.
As a further improvement of the first aspect of the invention: when the slurry contains calcium sulfate powder, the weight parts ratio of the carbon powder to the calcium sulfate powder to the tar to the water is 100: (7-11): (50-60): (15-30).
As a further improvement of the first aspect of the invention: the preparation of the slurry comprises the following steps: putting the carbon powder and the calcium sulfate powder into a stirrer to stir for 5-20 minutes to obtain a mixture; putting the mixture into a kneader, adding tar and kneading for 5-15 minutes, adding pure water and kneading for 10-20 minutes to obtain the slurry.
As a further improvement of the first aspect of the invention: the carbonization treatment is carried out for 1 to 3 hours under the inert atmosphere and at the temperature of 500 to 600 ℃; the activation treatment is carried out for 2-4 hours in an activation atmosphere at 800-1000 ℃.
As a further improvement of the first aspect of the invention: the slurry is extruded into spheres, columns or honeycombs.
In order to achieve the above object, according to a second aspect of the present invention, there is provided a bamboo activated carbon, comprising:
the bamboo activated carbon is prepared by the preparation method of the first aspect; BET specific surface area is not less than 1201.37 square meters/gram.
The invention has the following advantages:
(1) The invention uses the diffusion of carbon dioxide generated by the reaction of calcium sulfate and carbon at high temperature to form rich pores in the material for pore-forming, the used calcium sulfate is a raw material which is friendly to human body and environment, has abundant resources and low price, the porosity can be obviously increased by a small amount of calcium sulfate, and the generated small amount of calcium sulfide is further converted into calcium oxide tightly combined with a carbon matrix in the subsequent high-temperature activation process, so that the calcium sulfate can be used as an adsorbent without subsequent treatment.
(2) When the calcium sulfate adopts whisker powder, the whisker and other components are mutually entangled to form a three-dimensional net structure, so that the use of forming additives can be reduced, and the mechanical strength and the porosity can be both achieved. When the desulfurization byproduct gypsum is adopted as the calcium sulfate, the high-value secondary recycling of the desulfurization byproduct gypsum can be realized, and the technical problem that the application of the existing gypsum method is limited due to high solid waste yield is solved. In order to obtain the best performance and reduce the use cost of the calcium sulfate, it is preferable to use the desulfurization byproduct gypsum as the powder and the calcium sulfate whisker powder as the slurry.
(3) In the carbonization process, calcium sulfate and carbon can react to form pores, the original carbonization process is not changed, and the activation effect and activation efficiency can be remarkably improved when the precursor with certain porosity is activated again.
(4) Because the fresh bamboo powder has stronger toughness and is difficult to crush into smaller granularity, the carbon powder which is ground after carbonization is generally used as a pulping raw material, but the carbon powder has higher hardness and longer grinding time. In the invention, when the fresh bamboo powder and the calcium sulfate are carbonized for the first time, the carbon powder with a certain porosity can be obtained, the hardness of the carbon powder is reduced, and the carbon powder is convenient to grind into finer powder, so that the homogeneity of slurry is improved, the kneading time is shortened, the secondary carbonization and activation efficiency is improved, and the production efficiency is improved.
(5) In the kneading process, firstly, the carbon powder and the calcium sulfate powder are fully and uniformly mixed and then kneaded, so that the calcium sulfate and the carbon can fully react, the uniformity of pores is improved, and the mechanical strength is improved.
Therefore, the preparation method of the bamboo activated carbon with high specific surface area has the advantages of simple and easily controlled process, high production efficiency, green and environment-friendly raw materials and low cost, and can be implemented by directly adopting equipment of the traditional process. The bamboo activated carbon prepared by the preparation method mainly contains micropores, has developed and uniform pores, has a specific surface area of more than 1201.37 square meters per gram, has good mechanical strength, has excellent adsorption performance and long service life when being used as an adsorbent, and can be used as a carrier of a catalyst due to the high specific surface area, so that the preparation method of the bamboo activated carbon with high specific surface area and the bamboo activated carbon have extremely strong practicability.
Additional aspects and advantages of the inventive embodiments provided herein will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the inventive embodiments provided herein.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and, together with the description, serve to explain, without undue limitation, the embodiments of the invention.
Fig. 1 is a nitrogen adsorption and desorption graph of the bamboo activated carbon of example 7.
Fig. 2 is a graph showing pore size distribution of the bamboo activated carbon of example 7.
Fig. 3 is a scanning electron microscope image of the bamboo activated carbon of example 7.
Fig. 4 is a topography of a calcium sulfate whisker.
Detailed Description
The following provides a clear and complete description of the inventive embodiments provided in this specification in connection with the accompanying drawings. Those skilled in the art will be able to implement the embodiments of the invention provided herein based on these descriptions. Before describing embodiments of the invention provided in this specification with reference to the drawings, it should be noted in particular that:
in the embodiments of the invention provided in the present specification, the technical solutions and technical features provided in the respective sections including the following description may be combined with each other without conflict.
Moreover, the embodiments of the invention provided in the present specification referred to in the following description are generally only some, but not all, embodiments of the invention provided in the present specification, and therefore, all other embodiments obtained by a person having ordinary skill in the art based on the embodiments of the invention provided in the present specification without making any inventive effort shall fall within the scope of protection of the embodiments of the invention provided in the present specification.
Terms and units in the examples of the invention provided in the present specification: the terms "comprising," "including," "having," and any variations thereof, in the description and claims of embodiments of the invention and in the relevant parts, are intended to cover a non-exclusive inclusion. In addition, other related terms and units in the embodiments of the invention provided in the present specification can be reasonably interpreted based on the related contents of the embodiments of the invention provided in the present specification.
Example 1
The preparation method of the bamboo activated carbon with the high specific surface area comprises the following steps:
(1) Carbonizing fresh bamboo powder for 2 hours at 600 ℃ in nitrogen atmosphere to obtain carbon powder.
(2) Extruding and molding slurry comprising carbon powder, calcium sulfate powder, tar and water to obtain a columnar green body with the diameter of 4 mm; wherein,,
the calcium sulfate powder is calcium sulfate whisker powder and mainly comprises fibers with the length of 100-460 mu m and the width of 12-25 mu m.
The weight portion ratio of the carbon powder to the calcium sulfate powder to the tar to the water is 100:7:55:25.
the preparation of the slurry comprises the following steps: putting the carbon powder and the calcium sulfate powder into a stirrer to stir for 10 minutes to obtain a mixture; the mixture was put into a kneader at a rotational speed of 30 rpm, tar was first added and kneaded for 10 minutes, and then pure water was added and kneaded for 15 minutes again to obtain a slurry.
The granularity of the carbon powder is 200 meshes.
(3) Carbonizing the blank for 1 hour at 600 ℃ in nitrogen atmosphere to obtain a precursor.
(4) And (3) introducing 40 ml/h of water vapor into every 100 g of precursor, and performing activation treatment on the precursor for 3 hours at 900 ℃ in the water vapor atmosphere to obtain the bamboo activated carbon with high specific surface area.
Example 2
The preparation method of this example has the following differences compared with example 1: the weight portion ratio of the carbon powder to the calcium sulfate powder to the tar to the water is 100:9:55:25.
example 3
The preparation method of this example has the following differences compared with example 1: the weight portion ratio of the carbon powder to the calcium sulfate powder to the tar to the water is 100:11:55:25.
example 4
The preparation method of this example has the following differences compared with example 1: the calcium sulfate powder is desulfurization byproduct gypsum.
Example 5
The preparation method of the bamboo activated carbon with the high specific surface area comprises the following steps:
(1) Carbonizing powder comprising fresh bamboo powder and calcium sulfate powder for 2 hours at 600 ℃ in nitrogen atmosphere to obtain carbon powder; wherein the calcium sulfate powder is calcium sulfate whisker powder and mainly comprises fibers with the length of 100-460 mu m and the width of 12-25 mu m; the weight of the calcium sulfate powder is 10% of the weight of the fresh bamboo powder.
(2) Extruding and molding slurry comprising carbon powder, tar and water to obtain a columnar blank body with the diameter of 4 mm; wherein,,
the weight portion ratio of the carbon powder, the tar and the water is 100:55:25.
the preparation of the slurry comprises the following steps: the carbon powder was put into a kneader at a rotational speed of 30 rpm, and the tar was first added and kneaded for 10 minutes, and then pure water was added and kneaded for 15 minutes again, to thereby obtain a slurry.
The granularity of the carbon powder is 200 meshes.
(3) Carbonizing the blank for 1 hour at 600 ℃ in nitrogen atmosphere to obtain a precursor.
(4) And (3) introducing 40 ml/h of water vapor into every 100 g of precursor, and performing activation treatment on the precursor for 3 hours at 900 ℃ in the water vapor atmosphere to obtain the bamboo activated carbon with high specific surface area.
Example 6
The preparation method of this example has the following differences compared with example 5: the weight of the calcium sulfate powder is 12% of the weight of the fresh bamboo powder.
Example 7
The preparation method of this example has the following differences compared with example 5: the weight of the calcium sulfate powder is 15% of the weight of the fresh bamboo powder.
Example 8
The preparation method of this example has the following differences compared with example 5: the calcium sulfate powder is desulfurization byproduct gypsum.
Example 9
The preparation method of the bamboo activated carbon with the high specific surface area comprises the following steps:
(1) Carbonizing powder comprising fresh bamboo powder and calcium sulfate powder for 2 hours at 600 ℃ in nitrogen atmosphere to obtain carbon powder; wherein the weight of the calcium sulfate powder is 12% of the weight of the fresh bamboo powder.
(2) Extruding and molding slurry comprising carbon powder, calcium sulfate powder, tar and water to obtain a columnar green body with the diameter of 4 mm; wherein,,
the weight portion ratio of the carbon powder to the calcium sulfate powder to the tar to the water is 100:9:55:25.
the calcium sulfate powder in the steps (1) and (2) is calcium sulfate whisker powder, and mainly comprises fibers with the length of 100-460 mu m and the width of 12-25 mu m.
The preparation of the slurry comprises the following steps: putting the carbon powder and the calcium sulfate powder into a stirrer to stir for 10 minutes to obtain a mixture; the mixture was put into a kneader at a rotational speed of 30 rpm, tar was first added and kneaded for 10 minutes, and then pure water was added and kneaded for 15 minutes again to obtain a slurry.
The granularity of the carbon powder is 200 meshes.
(3) Carbonizing the blank for 1 hour at 600 ℃ in nitrogen atmosphere to obtain a precursor.
(4) And (3) introducing 40 ml/h of water vapor into every 100 g of precursor, and performing activation treatment on the precursor for 3 hours at 900 ℃ in the water vapor atmosphere to obtain the bamboo activated carbon with high specific surface area.
Example 10
The preparation method of this example has the following differences compared with example 9: the calcium sulfate powder in the powder is desulfurization byproduct gypsum.
Example 11 (control)
The preparation method of the bamboo activated carbon with the high specific surface area comprises the following steps:
(1) Carbonizing fresh bamboo powder for 2 hours at 600 ℃ in nitrogen atmosphere to obtain carbon powder.
(2) Extruding and molding slurry comprising carbon powder, tar and water to obtain a columnar blank body with the diameter of 4 mm; wherein,,
the weight portion ratio of the carbon powder, the tar and the water is 100:55:25.
the preparation of the slurry comprises the following steps: the carbon powder was put into a kneader at a rotational speed of 30 rpm, and the tar was first added and kneaded for 10 minutes, and then pure water was added and kneaded for 15 minutes again, to thereby obtain a slurry.
The granularity of the carbon powder is 200 meshes.
(3) Carbonizing the blank for 1 hour at 600 ℃ in nitrogen atmosphere to obtain a precursor.
(4) And (3) introducing 40 ml/h of water vapor into every 100 g of precursor, and performing activation treatment on the precursor for 3 hours at 900 ℃ in a water vapor atmosphere to obtain the activated carbon.
The specific surface area and the average pore diameter of the bamboo activated carbon of examples 1 to 11 were tested by using "measurement of pore volume and specific surface area of coal particle activated carbon test method" (GB/T7702.20-2008), and the test results are shown in Table 1.
As can be seen from table 1, compared with example 11, the specific surface area of the bamboo activated carbon of examples 1 to 10 is significantly increased, which indicates that the use of calcium sulfate in the present invention can significantly increase the porosity, but can retain the microporous structure, and has good adsorption performance in practical application, and no abrasion and breakage occur even after long-term use.
Fig. 1 is a nitrogen adsorption and desorption curve of the bamboo activated carbon of example 7. Fig. 2 is a pore size distribution curve of the bamboo activated carbon of example 7, which was obtained by testing a high performance specific surface area and a micro pore analyzer (model number BSD-PM) of Bei Shide instrument technology (beijing) limited.
As shown in fig. 1, the bamboo activated carbon shows a standard type i isotherm, i.e., langmuir isotherm, which is typical of microporous materials. As shown in figure 2, the pore diameter of the bamboo activated carbon is mainly distributed below 2nm, and the bamboo activated carbon shows obvious micropore material characteristics.
Fig. 3 is a scanning electron microscope image of the bamboo activated carbon of example 7.
As shown in FIG. 3, the bamboo activated carbon has a loose porous three-dimensional network structure, so that the bamboo activated carbon has high specific surface area and air permeability.
The preparation of the calcium sulfate whisker may, but is not limited to, employ the following steps:
1.625 mol/l of 160 ml of sulfuric acid was added to 80 ml of an aqueous dispersion of calcium oxide (20 g), and the precipitate formed was collected, washed and dried; dispersing 3.513 g of precipitate in 500 ml of sulfuric acid, carrying out water bath and stirring treatment at 80 ℃, standing for 20 hours at room temperature after the precipitate is completely dissolved, and then collecting, washing and drying the separated precipitate to obtain the calcium sulfate whisker.
Fig. 4 is a topography of a calcium sulfate whisker.
As can be seen from FIG. 4, the calcium sulfate whisker powder is mainly composed of fibers having a length of 100 to 460 μm and a width of 12 to 25. Mu.m.
The desulfurization byproduct gypsum is a byproduct of gypsum desulfurization, and the principle of gypsum desulfurization is as follows: limestone or lime is used as a desulfurization absorbent, the limestone is crushed and ground into powder and is mixed with water to be stirred into absorption slurry, or the lime powder is digested and then added with water to be prepared into absorbent slurry; the absorption slurry is contacted and mixed with the flue gas to be desulfurized, sulfur dioxide in the flue gas is chemically reacted with calcium carbonate in the slurry and blown oxidized air so as to be removed, and the final reaction product is gypsum. When the desulfurization byproduct gypsum is applied to the invention, the gypsum is ground into powder and then screened by a 200-mesh screen for use.
The above description has been made of the contents of the embodiments of the invention provided in the present specification. Those skilled in the art will be able to implement the embodiments of the invention provided herein based on these descriptions. Based on the foregoing of the inventive embodiments provided herein, all other preferred embodiments and examples, which a person of ordinary skill in the art would obtain without making any inventive effort, shall fall within the scope of the inventive embodiments provided herein.
Claims (6)
1. The preparation method of the bamboo activated carbon with high specific surface area is characterized by comprising the following steps: the method comprises the following steps:
(1) Carbonizing a powder body comprising fresh bamboo powder to obtain carbon powder;
(2) Extruding and molding slurry comprising carbon powder, tar and water to obtain a blank;
(3) Carbonizing the blank to obtain a precursor;
(4) Activating the precursor to obtain the bamboo activated carbon with high specific surface area;
wherein the powder and/or slurry further comprises calcium sulfate powder;
the calcium sulfate powder is calcium sulfate whisker powder;
the calcium sulfate whisker powder mainly comprises fibers with the length of 100-460 mu m and the width of 12-25 mu m;
when the slurry contains calcium sulfate powder, the weight parts ratio of the carbon powder to the calcium sulfate powder to the tar to the water is 100: (7-11): (50-60): (15-30);
the carbonization treatment is carried out for 1 to 3 hours under the inert atmosphere and at the temperature of 500 to 600 ℃; the activation treatment is carried out for 2-4 hours in an activation atmosphere at 800-1000 ℃.
2. The method for preparing the bamboo activated carbon with high specific surface area according to claim 1, which is characterized in that: the preparation of the calcium sulfate whisker comprises the following steps: adding sulfuric acid into the calcium oxide aqueous dispersion, and then collecting, washing and drying the generated precipitate; dispersing the precipitate in sulfuric acid, heating, standing at room temperature until the precipitate is separated out after the precipitate is completely dissolved, and collecting, washing and drying the separated precipitate to obtain the calcium sulfate whisker.
3. The method for preparing the bamboo activated carbon with high specific surface area according to claim 1, which is characterized in that: when the powder contains calcium sulfate powder, the weight of the calcium sulfate powder is 10-15% of that of the fresh bamboo powder.
4. The method for preparing the bamboo activated carbon with high specific surface area according to claim 1, which is characterized in that: the preparation of the slurry comprises the following steps: putting the carbon powder and the calcium sulfate powder into a stirrer to stir for 5-20 minutes to obtain a mixture; putting the mixture into a kneader, adding tar and kneading for 5-15 minutes, adding pure water and kneading for 10-20 minutes to obtain the slurry.
5. The method for preparing the bamboo activated carbon with high specific surface area according to claim 1, which is characterized in that: the slurry is extruded into spheres, columns or honeycombs.
6. Bamboo activated carbon, its characterized in that: prepared by the preparation method of any one of claims 1 to 5; BET specific surface area of not less than 1201.37m 2 /g。
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