CN116730339A - Novel wood columnar activated carbon harmless preparation equipment and process thereof - Google Patents
Novel wood columnar activated carbon harmless preparation equipment and process thereof Download PDFInfo
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- CN116730339A CN116730339A CN202310774236.XA CN202310774236A CN116730339A CN 116730339 A CN116730339 A CN 116730339A CN 202310774236 A CN202310774236 A CN 202310774236A CN 116730339 A CN116730339 A CN 116730339A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 238000002360 preparation method Methods 0.000 title claims abstract description 80
- 239000002023 wood Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000008569 process Effects 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 230000003213 activating effect Effects 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- 239000002028 Biomass Substances 0.000 claims abstract description 25
- 230000004913 activation Effects 0.000 claims abstract description 23
- 239000012153 distilled water Substances 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 16
- 239000000853 adhesive Substances 0.000 claims abstract description 14
- 230000001070 adhesive effect Effects 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 12
- 239000012190 activator Substances 0.000 claims abstract description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 24
- 238000001994 activation Methods 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 239000001569 carbon dioxide Substances 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 6
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 6
- 229920000877 Melamine resin Polymers 0.000 claims description 6
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 6
- 239000001099 ammonium carbonate Substances 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 6
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- NVJCKICOBXMJIJ-UHFFFAOYSA-M potassium;1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylate Chemical compound [K+].C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C([O-])=O NVJCKICOBXMJIJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000005995 Aluminium silicate Substances 0.000 claims description 5
- 240000008042 Zea mays Species 0.000 claims description 5
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 5
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims description 5
- 239000010426 asphalt Substances 0.000 claims description 5
- 235000005822 corn Nutrition 0.000 claims description 5
- 239000012043 crude product Substances 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 2
- 244000105624 Arachis hypogaea Species 0.000 claims description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 2
- 235000018262 Arachis monticola Nutrition 0.000 claims description 2
- 244000060011 Cocos nucifera Species 0.000 claims description 2
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 2
- 229920000742 Cotton Polymers 0.000 claims description 2
- 240000007049 Juglans regia Species 0.000 claims description 2
- 235000009496 Juglans regia Nutrition 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 239000011280 coal tar Substances 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 235000020232 peanut Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 235000020234 walnut Nutrition 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 125000004432 carbon atom Chemical group C* 0.000 abstract description 3
- 239000001913 cellulose Substances 0.000 abstract description 2
- 229920002678 cellulose Polymers 0.000 abstract description 2
- 238000005470 impregnation Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000012855 volatile organic compound Substances 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 19
- 238000001179 sorption measurement Methods 0.000 description 18
- 238000003795 desorption Methods 0.000 description 6
- 238000003912 environmental pollution Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000010902 straw Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 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
- 230000007547 defect Effects 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005303 weighing 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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- 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
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Carbon And Carbon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The application discloses novel wood columnar activated carbon harmless preparation equipment and process in the technical field of activated carbon preparation, wherein the equipment comprises the following components in parts by weight: 60-80 parts of biomass raw material, 2.5-5 parts of activating agent, 120-150 parts of distilled water and 5-9 parts of adhesive. The application reduces the crystallinity of cellulose in the raw material by ultrasonic treatment, effectively improves the impregnation efficiency of the activator, generates a plurality of micropores by using a physical activation method, simultaneously carries out chemical activation, and decomposes the activator and reacts CO and CO with carbon atoms 2 、H 2 O、NH 3 Equal small molecular gas expansionMacropores, NH 3 Simultaneously carrying out nitrogen doping, K is higher than 700 DEG C 2 K steam generated by the reaction of O and C can be inserted into the carbon array to enlarge the pores. In conclusion, the method has the advantages that the purposes of high product yield, large specific surface area and developed pore structure are achieved, the pore structure can be effectively regulated and controlled, the pollution to the environment is reduced, and the nitrogen doping can enhance the active site and electronegativity of the activated carbon, so that the purifying effect on volatile organic compounds is improved.
Description
Technical Field
The application belongs to the technical field of activated carbon preparation, and particularly relates to novel wood columnar activated carbon harmless preparation equipment and a process thereof.
Background
The active carbon is a carbon material with a porous and microcrystalline structure, has a very developed pore structure and a huge specific surface area, and has the dual characteristics of physical adsorption and chemical adsorption. Therefore, as an excellent adsorbent, the activated carbon can selectively adsorb colored molecules, organic substances and the like in liquid phase and gas phase so as to achieve the effects of decolorization and refining, deodorization and disinfection, decontamination and purification and the like. The activated carbon has wide application and plays an important role in different fields of medicine, metallurgy, food, chemical industry, military, environmental protection and the like.
At present, the activation process of the activated carbon is mainly divided into a physical activation method and a chemical activation method: the physical activation is generally to carbonize the raw materials firstly, then activate the raw materials by taking carbon dioxide, water vapor and the like as activating mediums, the physical activation technology is simple and convenient to operate, less in environmental pollution and lower in product yield; the chemical activation method generally adopts chemical substances such as phosphoric acid, zinc chloride, potassium carbonate, sodium hydroxide, potassium hydroxide and the like as an activating agent, and the prepared activated carbon has larger specific surface area and rich pore structure, however, the chemical activation method has the problems of consuming a large amount of activating agent, having higher environmental pollution degree and the like in the preparation process.
Disclosure of Invention
Aiming at the situation, the application provides novel wood column-shaped active carbon harmless preparation equipment and a process thereof for overcoming the defects of the prior art, and aims to solve the problems of low physical activation yield, large consumption of activating agent in chemical activation and environmental pollution.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows: washing biomass raw materials with water to remove impurities, drying, crushing, performing ultrasonic treatment by utilizing ultrasonic waves, adding the biomass raw materials and an activating agent into a stirring device together, uniformly mixing, adding distilled water, uniformly stirring, introducing nitrogen, heating and carbonizing, stopping introducing nitrogen, continuously heating, introducing carbon dioxide/water vapor mixed gas for activation, washing crude products with distilled water and dilute hydrochloric acid successively to remove ash and residual activating agent, repeatedly washing with distilled water until filtrate is neutral, mixing and stirring the filtrate with an adhesive, adding an extruder for extrusion into a column shape, and then placing the column shape into a dryer for drying to obtain the novel wood column-shaped active carbon.
Further, the novel wood columnar activated carbon comprises the following components in parts by weight: 60-80 parts of biomass raw materials, 8-12 parts of activating agents, 120-150 parts of distilled water and 5-9 parts of adhesives.
The activator comprises the following components in parts by weight: 35-40 parts of potassium abietate, 15-20 parts of ammonium bicarbonate and 20-25 parts of melamine.
Further, the biomass raw material is selected from one of peanut shells, cotton, wood chips, corn stalks, walnut shells and coconut shells.
Further, the ultrasonic treatment time is 2-4h, the ultrasonic frequency is 50-80kHz, and the power is 180-250W.
Further, the mass ratio of the biomass raw material to the activating agent is 2.5-4.0:1, and the mass ratio of the activating agent to the distilled water is 0.4-0.6:1.
Further, the nitrogen flow is 0.3-0.6L/min, the carbonization temperature is 550-600 ℃, and the heat preservation time is 1.5-3h.
Further, the flow rate of the carbon dioxide/water vapor mixed gas is 0.5-1.0L/min, the activation temperature is 700-750 ℃, and the heat preservation time is 1.5-3h.
Further, the adhesive is selected from one or more of asphalt powder, coal tar, kaolin and starch; the drying temperature is 110-140 ℃ and the drying time is 10-14h.
Further, the application also provides novel wood columnar activated carbon harmless preparation equipment, which comprises the following steps: the utility model discloses a preparation device, including preparation device body, material inlet, belt, motor support, driven gear wheel, motor support, material inlet, material outlet, material inlet and material outlet, the material inlet is located preparation device body one side top, the material outlet is located preparation device body opposite side below, the material inlet below is located to the air heater, preparation device body sprocket encircles and locates preparation device body middle part, preparation device body support locates preparation device body below, stirring vane locates preparation device body inside, driven gear is connected through the meshing with preparation device body sprocket, driven gear pivot is fixed to be set up on driven gear, driven gear runner is fixed to be set up in driven gear pivot, driven device fixed disk locates driven gear runner below and is fixed to be located on the preparation device body support, the belt is located on driven gear runner and the motor carousel, the motor support is located the motor below and is fixed to be located on the preparation device body support.
The beneficial effects obtained by the application are as follows:
(1) The crystallinity of cellulose in the biomass raw material is reduced through ultrasonic treatment, so that the impregnation efficiency of the activating agent can be effectively improved;
(2) Physical activation by steam and carbon dioxide and reaction with carbon atoms in the carbon material to generate a plurality of micropores;
(3) The organic part of the potassium abietate after being heated can be used as a carbon source to prepare active carbon, and the inorganic part is decomposed to generate K 2 CO 3 、K 2 O,CO 2 The reaction of the intermediate products with the C atoms on the surface of the biomass raw material to produce CO and CO 2 、H 2 O, ammonium bicarbonate and melamine are decomposed to produce CO and CO 2 、H 2 O、NH 3 These gases, when they largely escape the carbon surface, create a large number of pores, while NH 3 Can carry out nitrogen doping on the activated carbon and CO 2 And the water vapor can act as a physical activation to enlarge the pores, and the generated CO is opposite to CO 2 Plays a certain role in dilution and prevents CO 2 Pore collapse during pore formation and reaming, and effectively reduces burning loss of carbon, K at above 700 DEG C 2 K steam generated by the reaction of O and C can be inserted into the carbon array, and the micropore structure can be further enlarged.
By combining the advantages, the application realizes the purposes of high product yield, large specific surface area and developed pore structure, can effectively regulate and control the pore structure, avoids using a high-corrosivity activating agent, reduces the environmental pollution, and can enhance the active site and electronegativity of the active carbon by nitrogen doping so as to improve the purifying effect on volatile organic matters.
Drawings
FIG. 1 is SO for the different activated carbons of examples 1-3 and comparative examples 1-3 2 A result graph of the adsorption curve;
FIG. 2 is SO for the different activated carbons of examples 1-3 and comparative examples 1-3 2 A result graph of the desorption curve;
FIG. 3 is a graph showing the toluene adsorption results of the different activated carbons of example 1 and comparative examples 1 to 3;
FIG. 4 is an SEM image of example 1 and comparative examples 1-3;
FIG. 5 is a perspective view of a novel wood-column-shaped activated carbon harmless preparation device provided by the application;
FIG. 6 is an enlarged view at B in FIG. 5;
FIG. 7 is a front view of a novel wood-column-shaped activated carbon harmless preparation device provided by the application;
fig. 8 is a cross-sectional view of A-A of fig. 7.
The accompanying drawings are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate the application and together with the embodiments of the application, serve to explain the application.
Wherein, 1, a preparation device body, 2, a raw material inlet, 3, a hot air blower, 4, a preparation device body chain wheel, 5, a preparation device body bracket, 6, stirring blades, 7 and a driven gear, 8, driven gear rotating shafts, 9, driven gear rotating wheels, 10, driven device fixing discs, 11, belts, 12, motor rotating discs, 13, motors, 14, motor supports, 15 and a material outlet.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the application; all other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present application. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the application.
The experimental methods in the following examples are all conventional methods unless otherwise specified; the test materials used in the examples described below, unless otherwise specified, were purchased from commercial sources.
Example 1
Novel wood columnar activated carbon harmless preparation equipment and process thereof
The novel wood columnar activated carbon comprises the following components in parts by weight: 60 parts of biomass raw material, 8 parts of activating agent, 120 parts of distilled water and 9 parts of adhesive.
The activator comprises the following components in parts by weight: 35 parts of potassium abietate, 18 parts of ammonium bicarbonate and 22 parts of melamine.
Further, the biomass raw material is corn straw; the ultrasonic treatment time is 4 hours, the ultrasonic frequency is 50kHz, and the power is 200W; the mass ratio of the biomass raw material to the activating agent is 2.5:1; the mass ratio of the activating agent to distilled water is 0.5:1; the nitrogen flow is 0.3L/min; the carbonization temperature is 550 ℃, and the heat preservation time is 2.0h; the flow rate of the carbon dioxide/water vapor mixed gas is 0.5L/min; the activation temperature is 720 ℃, and the heat preservation time is 1.5h; the adhesive is prepared by mixing asphalt powder and kaolin according to a mass ratio of 1:1; the drying temperature is 120 ℃, and the drying time is 12 hours.
The preparation method of the novel wood columnar activated carbon comprises the following steps: washing biomass raw materials with water to remove impurities, drying at 120 ℃ for 12 hours, crushing, sieving with a 200-mesh screen, carrying out ultrasonic treatment by utilizing ultrasonic waves, adding the crushed biomass raw materials and an activating agent into a stirring device together according to a proportion, uniformly mixing, adding distilled water, stirring until the mixture is fully mixed, introducing nitrogen, heating and carbonizing at a heating rate of 10 ℃/min, continuously heating at a heating rate of 10 ℃/min, stopping introducing nitrogen, introducing carbon dioxide/steam mixed gas for activation, washing the obtained crude product by using distilled water and 0.1mol/L dilute hydrochloric acid in sequence to remove ash and residual activating agent, repeatedly washing the crude product by using distilled water until filtrate is neutral, mixing and stirring the crude product and the adhesive, adding the mixture into an extruder, extruding the mixture into a column, and then placing the column into a dryer for drying to obtain the novel wood column-shaped activated carbon.
The preparation apparatus as described in fig. 4 to 7 includes: the material inlet 2 is arranged above one side of the preparation device body 1, the material outlet 15 is arranged below the other side of the preparation device body 1, the air heater 3 is arranged below the material inlet 2, the preparation device body chain wheel 4 is arranged around the middle of the preparation device body 1, the preparation device body bracket 5 is arranged below the preparation device body 1, the stirring blades 6 are arranged inside the preparation device body 1, the driven gear 7 is connected with the preparation device body chain wheel 4 through meshing, the driven gear rotating shaft 8 is fixedly arranged on the driven gear 7, the driven gear rotating wheel 9 is fixedly arranged on the driven gear rotating shaft 8, the driven device fixing disc 10 is arranged below the driven gear rotating wheel 9 and is fixedly arranged on the preparation device body bracket 5, the belt 11 is arranged on the driven gear rotating wheel 9 and the motor rotating disc 12, the motor 13 is connected on the motor rotating disc 12, and the motor bracket 14 is arranged below the motor 13 and is fixedly arranged on the preparation device body bracket 5.
Working principle: the motor 13 and the air heater 3 are started, the motor 13 drives the motor turntable 12 to rotate, the motor turntable 12 drives the driven gear runner 9, the driven gear rotating shaft 8 and the driven gear 7 to rotate through the belt 11, the driven gear 7 drives the preparation device body sprocket 4 to rotate through meshing with the preparation device body sprocket 4, the preparation device body sprocket 4 drives the preparation device body 1 to rotate, and the air heater 3 brings heat into the preparation device body 1 to stir and dry raw materials.
Example 2
Novel wood columnar activated carbon harmless preparation equipment and process thereof
The novel wood columnar activated carbon comprises the following components in parts by weight: 80 parts of biomass raw material, 12 parts of activating agent, 120 parts of distilled water and 5 parts of adhesive.
The activator comprises the following components in parts by weight: 40 parts of potassium abietate, 20 parts of ammonium bicarbonate and 25 parts of melamine.
Further, the biomass raw material is corn straw; the ultrasonic treatment time is 2 hours, the ultrasonic frequency is 50kHz, and the power is 200W; the mass ratio of the biomass raw material to the activating agent is 4:1; the mass ratio of the activating agent to distilled water is 0.5:1; the nitrogen flow is 0.3L/min; the carbonization temperature is 600 ℃, and the heat preservation time is 2.0h; the flow rate of the carbon dioxide/water vapor mixed gas is 1.0L/min; the activation temperature is 750 ℃, and the heat preservation time is 1.5h; the adhesive is prepared by mixing asphalt powder and kaolin according to a mass ratio of 1:1; the drying temperature is 120 ℃, and the drying time is 12 hours.
The novel wood columnar activated carbon harmless preparation equipment and the process thereof are shown in an example 1.
Example 3
Novel wood columnar activated carbon harmless preparation equipment and process thereof
The novel wood columnar activated carbon comprises the following components in parts by weight: 75 parts of biomass raw material, 10 parts of activating agent, 125 parts of distilled water and 6.5 parts of adhesive.
The activator comprises the following components in parts by weight: 380 parts of potassium abietate, 15 parts of ammonium bicarbonate and 24 parts of melamine.
Further, the biomass raw material is corn straw; the ultrasonic treatment time is 3 hours, the ultrasonic frequency is 50kHz, and the power is 200W; the mass ratio of the biomass raw material to the activating agent is 3.5:1; the mass ratio of the activating agent to distilled water is 0.6:1; the nitrogen flow is 0.5L/min; the carbonization temperature is 600 ℃, and the heat preservation time is 2.5 hours; the flow rate of the carbon dioxide/water vapor mixed gas is 0.8L/min; the activation temperature is 750 ℃, and the heat preservation time is 2 hours; the adhesive is prepared by mixing asphalt powder and kaolin according to a mass ratio of 1:1; the drying temperature is 110 ℃, and the drying time is 12 hours.
The novel wood columnar activated carbon harmless preparation equipment and the process thereof are shown in an example 1.
Comparative example 1
This comparative example provides a wood-column-shaped activated carbon harmless preparation apparatus and a process thereof, which are different from example 1 in that the biomass raw material is not subjected to ultrasonic treatment, and the remaining components, component contents, and preparation steps are the same as example 1.
Comparative example 2
The comparative example provides a wood-column-shaped activated carbon harmless preparation device and a process thereof, which are different from example 1 in that the wood-column-shaped activated carbon is directly carbonized without mixing with an activating agent and water, and is activated without continuously heating up and introducing a carbon dioxide/water vapor mixed gas, and the rest components, component contents and preparation steps are the same as those of example 1.
Comparative example 3
The comparative example provides a wood column-shaped activated carbon harmless preparation device and a process thereof, which are different from example 1 in that nitrogen is not introduced to carry out carbonization, the temperature is directly raised to an activation temperature, and carbon dioxide/water vapor mixed gas is introduced to carry out activation, and other components, component contents and preparation steps are the same as example 1.
Analysis of results
SO was performed on examples 1-3 and comparative examples 1-3 with reference to GB/T320202.4-2013 2 Adsorption and desorption detection, placing the sample into an adsorption testing device after being sufficiently dried, controlling the gas flow of a gas cylinder by a flowmeter during adsorption, wherein the components of the mixed gas are SO 2 (volume fraction 0.1%), O 2 (volume fraction 6.4%), H 2 O (volume fraction 9.8%), N 2 (volume fraction was 83.7%), and the mixture was then adsorbed at 120.+ -. 5 ℃ for 4 hours. In desorption, the adsorbed sample is placed in N 2 And (3) desorbing for 2 hours at 400+/-5 ℃ in the atmosphere, recording data of tail gas by an analyzer, wherein the adsorption result is shown in figure 1, and the desorption result is shown in figure 2. As can be seen from fig. 1: the adsorption curves of the activated carbon have similar trend, and when the activated carbon prepared by the comparative example is used as an adsorbent, the activated carbon has similar trend to SO 2 The adsorption capacity is relatively poor, and the activated carbon subjected to ultrasonic treatment and physicochemical coupling activation in the examples has the effect of treating SO 2 The adsorption capacity of the catalyst is obviously improved. As can be seen from fig. 2: desorption yeast of several active carbonThe line trend was similar, and over 90% of the SO was released when desorption was carried out for 10min 2 And then release is slow, and the desulfurization value of the activated carbon in the examples is obviously improved compared with that of the comparative examples. Since the adsorption performance of the activated carbon is related to the number of micropores per unit volume, it is known that the number of micropores per unit volume of the activated carbon micropores in the examples exceeds that in the comparative example.
Toluene adsorption test was performed with reference to HJ584-2010 for example 1 and comparative examples 1-3, and the test method was: introducing air into toluene solution, and regulating flow rate by flow meter to obtain required concentration of about 750mg/m 3 And (3) introducing the toluene/air mixture into an adsorption device, weighing 0.4g of each of the example 1 and the comparative examples 1-3, carrying out dynamic adsorption of toluene at an air outlet, and detecting the toluene concentration at the air outlet, wherein a toluene adsorption result chart is shown in figure 3. As can be seen from fig. 3: the breakthrough time for toluene adsorption in example 1 was about 120min, which is higher than that in comparative examples 1-3, indicating that nitrogen doping of activated carbon is beneficial to adsorption of volatile organics by activated carbon.
In fig. 4, a-d are SEM images of example 1, comparative example 2 and comparative example 3, respectively, as can be seen from fig. 4: example 1 has a more dense, uniform, developed pore structure.
Although embodiments of the present application have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the application, the scope of which is defined in the appended claims and their equivalents.
The application and its embodiments have been described above with no limitation, and the application is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the application can be practiced without the specific details disclosed herein.
Claims (10)
1. A novel harmless preparation process of wood columnar activated carbon is characterized by comprising the following steps of: the preparation method of the novel wood columnar activated carbon comprises the following steps: washing biomass raw materials with water to remove impurities, drying, crushing, performing ultrasonic treatment by utilizing ultrasonic waves, adding the biomass raw materials and an activating agent into a stirring device together, uniformly mixing, adding distilled water, uniformly stirring, introducing nitrogen, heating and carbonizing, stopping introducing nitrogen, continuously heating, introducing carbon dioxide/water vapor mixed gas for activation, washing crude products with distilled water and dilute hydrochloric acid successively to remove ash and residual activating agent, repeatedly washing with distilled water until filtrate is neutral, mixing and stirring the filtrate with an adhesive, adding an extruder for extrusion into a column shape, and then placing the column shape into a dryer for drying to obtain the novel wood column-shaped active carbon.
2. The novel harmless preparation process of the wood columnar activated carbon, which is characterized by comprising the following steps of: the novel wood columnar activated carbon comprises the following components in parts by weight: 60-80 parts of biomass raw materials, 8-12 parts of activating agents, 120-150 parts of distilled water and 5-9 parts of adhesives.
3. The novel harmless preparation process of the wood columnar activated carbon, which is characterized by comprising the following steps of: the activator comprises the following components in parts by weight: 35-40 parts of potassium abietate, 15-20 parts of ammonium bicarbonate and 20-25 parts of melamine.
4. The novel wood-column-shaped activated carbon harmless preparation process according to claim 3, which is characterized in that: the biomass raw material is selected from one of peanut shells, cotton, wood chips, corn stalks, walnut shells and coconut shells.
5. The novel harmless preparation process of the wood columnar activated carbon, which is characterized by comprising the following steps of: the ultrasonic treatment time is 2-4h, the ultrasonic frequency is 50-80kHz, and the power is 180-250W.
6. The novel harmless preparation process of the wood columnar activated carbon, which is characterized in that: the mass ratio of the biomass raw material to the activating agent is 2.5-4.0:1.
7. The novel harmless preparation process of the wood columnar activated carbon, which is characterized by comprising the following steps of: the mass ratio of the activating agent to distilled water is 0.4-0.6:1.
8. The novel harmless preparation process of the wood columnar activated carbon, which is characterized in that: the nitrogen flow is 0.3-0.6L/min, the carbonization temperature is 550-600 ℃, and the heat preservation time is 1.5-3h; the flow rate of the carbon dioxide/water vapor mixture is 0.5-1.0L/min, the activation temperature is 700-750 ℃, and the heat preservation time is 1.5-3h.
9. The novel wood-column-shaped activated carbon harmless preparation device and the process thereof according to claim 8 are characterized in that: the adhesive is selected from one or more of asphalt powder, coal tar, kaolin and starch; the drying temperature is 110-140 ℃ and the drying time is 10-14h.
10. A preparation device of the novel wood-column-shaped activated carbon harmless preparation process according to claim 9, which is characterized in that: the preparation equipment comprises a preparation device body (1), a raw material inlet (2), a hot air blower (3), a preparation device body chain wheel (4), a preparation device body bracket (5), stirring blades (6), a driven gear (7), a driven gear rotating shaft (8), a driven gear rotating wheel (9), a driven device fixing disc (10), a belt (11), a motor rotating disc (12), a motor (13), a motor bracket (14) and a material outlet (15), wherein the raw material inlet (2) is arranged above one side of the preparation device body (1), the material outlet (15) is arranged below the other side of the preparation device body (1), the hot air blower (3) is arranged below the raw material inlet (2), the preparation device body chain wheel (4) is arranged around the middle of the preparation device body (1), the preparation device body bracket (5) is arranged below the preparation device body (1), the stirring blades (6) are arranged inside the preparation device body (1), the driven gear (7) is connected with the preparation device body chain wheel (4) through meshing, the driven gear (8) is fixedly arranged on the driven gear (7), the driven gear (9) is arranged on the driven gear (8) and the driven gear (8) is fixedly arranged on the rotating shaft, the driven device fixing disc (10) is arranged below the driven gear rotating wheel (9) and fixedly arranged on the preparation device body support (5), the belt (11) is arranged on the driven gear rotating wheel (9) and the motor rotating disc (12), the motor (13) is connected to the motor rotating disc (12), and the motor support (14) is arranged below the motor (13) and fixedly arranged on the preparation device body support (5).
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