CN113896194B - Preparation method of activated carbon and activated carbon - Google Patents
Preparation method of activated carbon and activated carbon Download PDFInfo
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- CN113896194B CN113896194B CN202111278693.7A CN202111278693A CN113896194B CN 113896194 B CN113896194 B CN 113896194B CN 202111278693 A CN202111278693 A CN 202111278693A CN 113896194 B CN113896194 B CN 113896194B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 192
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 145
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 145
- 241001330002 Bambuseae Species 0.000 claims abstract description 145
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 145
- 239000011425 bamboo Substances 0.000 claims abstract description 145
- 238000001035 drying Methods 0.000 claims abstract description 51
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000005539 carbonized material Substances 0.000 claims abstract description 46
- 239000003610 charcoal Substances 0.000 claims abstract description 45
- 240000003096 Chimonobambusa quadrangularis Species 0.000 claims abstract description 40
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910001425 magnesium ion Inorganic materials 0.000 claims abstract description 38
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 36
- 239000010865 sewage Substances 0.000 claims abstract description 34
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000002791 soaking Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000005520 cutting process Methods 0.000 claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 16
- 238000010000 carbonizing Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 230000003213 activating effect Effects 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000005406 washing Methods 0.000 claims description 22
- 230000004913 activation Effects 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- 230000008569 process Effects 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- 238000003763 carbonization Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 125000004122 cyclic group Chemical group 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000008399 tap water Substances 0.000 claims description 3
- 235000020679 tap water Nutrition 0.000 claims description 3
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 description 18
- 238000004519 manufacturing process Methods 0.000 description 14
- 244000005700 microbiome Species 0.000 description 10
- 239000011148 porous material Substances 0.000 description 10
- 230000003068 static effect Effects 0.000 description 8
- 238000001354 calcination Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 238000007598 dipping method Methods 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 6
- 230000002195 synergetic effect Effects 0.000 description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000011575 calcium Substances 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 229920002678 cellulose Polymers 0.000 description 5
- 230000000813 microbial effect Effects 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 241000195493 Cryptophyta Species 0.000 description 4
- 102000004190 Enzymes Human genes 0.000 description 4
- 108090000790 Enzymes Proteins 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000001814 pectin Substances 0.000 description 4
- 229920001277 pectin Polymers 0.000 description 4
- 235000010987 pectin Nutrition 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229920002488 Hemicellulose Polymers 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 2
- 241000192701 Microcystis Species 0.000 description 2
- 102000002262 Thromboplastin Human genes 0.000 description 2
- 108010000499 Thromboplastin Proteins 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000012190 activator Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229930002875 chlorophyll Natural products 0.000 description 2
- 235000019804 chlorophyll Nutrition 0.000 description 2
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 2
- LOHQECMUTAPWAC-UHFFFAOYSA-N coagulin Natural products C1C(C)=C(CO)C(=O)OC1C1(C)C(C2(C)CCC3C4(C(=O)CC=CC4=CCC43)C)(O)CCC24O1 LOHQECMUTAPWAC-UHFFFAOYSA-N 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000005429 filling process Methods 0.000 description 2
- -1 has macropores Chemical compound 0.000 description 2
- 239000004021 humic acid Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- 241000745988 Phyllostachys Species 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 210000004081 cilia Anatomy 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000009828 non-uniform distribution Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000003911 water pollution 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
- C01B32/318—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
- C01B32/336—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
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
Abstract
The application discloses a preparation method of active carbon and the active carbon, which is suitable for reducing or removing COD of sewage. The preparation method of the activated carbon comprises the following steps: taking bamboo tubes as raw materials, and cutting the bamboo tubes into bamboo rings with required lengths; soaking the bamboo rings in hydrochloric acid solution, cleaning with clear water, and drying; carbonizing the dried bamboo rings to obtain annular bamboo charcoal carbonized materials with the shape of the bamboo rings; immersing the annular bamboo charcoal carbonized material in a calcium-magnesium solution so as to adsorb calcium ions and magnesium ions; and (3) activating the annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions to obtain an active carbon product. The method fully utilizes the natural characteristics of the square bamboo to prepare the activated carbon for reducing the COD of the sewage, and simultaneously adopts a series of technical means to inhibit the defects of the square bamboo and further improve the sewage treatment advantages of the activated carbon.
Description
Technical Field
The application relates to a preparation method of active carbon and the active carbon.
Background
The water pollution degree can be roughly judged by using COD (Chemical Oxygen Demand ) index. The COD index indicates the content of reducing substances in water, which are mainly organic substances and exist as sulfite, nitrite, sulfide, etc. The higher the COD index of the water, the more oxygen is required in the degradation process. The higher the self-cleaning oxygen consumption of the water body is, the death of other organisms except microorganisms in the water body is caused, the blackening and the stinking of the water body are caused, and the surrounding environment is further influenced. The sewage treatment mainly reduces the COD index of the sewage.
In order to reduce the COD index of sewage, activated carbon can be used for adsorption. Currently, activated carbon for sewage treatment is mainly columnar activated carbon particles. The columnar activated carbon particles require special molding steps in the preparation process, so that the production cost is high. The columnar activated carbon particles can also increase water flow resistance and improve equipment energy consumption. In addition, the smaller the particle size of the columnar activated carbon particles is, the higher the removal rate of COD is, but the water flow resistance is correspondingly higher; the larger the particle diameter of the columnar activated carbon particles is, the lower the removal rate of COD tends to be.
Disclosure of Invention
The application aims to provide a preparation method of active carbon and the active carbon, which are suitable for reducing or removing COD of sewage.
According to a first aspect of the present application, there is provided a method for preparing activated carbon, comprising: taking bamboo tubes as raw materials, and cutting the bamboo tubes into bamboo rings with required lengths; soaking the bamboo rings in hydrochloric acid solution, cleaning with clear water, and drying; carbonizing the dried bamboo rings to obtain annular bamboo charcoal carbonized materials with the shape of the bamboo rings; immersing the annular bamboo charcoal carbonized material in a calcium-magnesium solution so as to adsorb calcium ions and magnesium ions; and (3) activating the annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions to obtain an active carbon product.
Fangzhu (academic name: chimonobambusa quadrangularis (Fenzi) Makino) is Gramineae, and the genus Phyllostachys is arbor-like. The rod is upright and can reach 8 meters, the internodes are in a rounded quadrangular shape, and the rings below the middle part of the rod are short and downward bent thorn-shaped aerial roots; sheath paper or thick paper, early falling property, short internode, cilia at sheath edge, clear longitudinal rib, purple small transverse pulse, and extremely obvious square shape; the sheath sheets are very small, conical, leaf sheath-shaped, smooth and hairless, sheath mouth-shaped Mao Zhili, smooth, short and truncated leaf tongue, thin leaf tissue, long elliptic needle-like, the upper surface is hairless, the lower surface is soft and the bract is less; the false small spike is slender, the lateral false small spike contains small flowers, and the small spike shaft is smooth and has no hair; the palace is in a needle shape, the palea paper is green, and the palea is equal to the palea in length; the scale is oval; the column head is feather-shaped. The square bamboo is representative of excellent bamboo shoots in Yibin areas, and the bamboo residues mainly comprise cellulose, hemicellulose, lignin, pectin and other organic matters, and pectin is decomposed at high temperature to generate a pore structure. The cut-off surface of the square bamboo tube is generally in a hollow annular structure. In addition, the long fibers which grow unidirectionally in the square bamboo can lead to strong anisotropy and uneven distribution of reinforcing phases, and meanwhile, cellulose is not bent strongly due to high temperature, so that the square bamboo can keep the original shape in the carbonization process, and the active carbon prepared by using the square bamboo as a raw material can be naturally molded, and the mechanical molding cost is reduced.
According to the preparation method of the activated carbon, firstly, the natural shape of the square bamboo tube is utilized to form the bamboo ring through cutting, and then the physical characteristics of the square bamboo are utilized (namely, long fibers growing in one direction in the square bamboo can cause strong anisotropy and non-uniform distribution of reinforcing phases, meanwhile, cellulose is not bent strongly due to high temperature, so that the square bamboo can keep the original shape in the carbonization process, the activated carbon prepared by using the square bamboo as a raw material can be naturally molded), and finally, the annular hollow activated carbon product is obtained without special molding steps. In addition, the activated carbon prepared from square bamboo is biological activated carbon, and sewage treatment can be performed by utilizing the synergistic effect of activated carbon adsorption and microbial organic decomposition in the activated carbon layer: on one hand, the active carbon concentrates organic matters on the surface of the carbon, improves the degradation efficiency of microorganisms, and on the other hand, the active carbon can maintain the activity of microorganisms by adsorbing dissolved oxygen in water, and reduces macromolecular organic pollutants in sewage through synergistic effect.
According to the preparation method of the activated carbon, the step of soaking the bamboo rings in the hydrochloric acid solution is adopted, on one hand, insoluble inorganic matters in the square bamboo and on the surface can be removed, the influence of external factors on the performance of the activated carbon is reduced, on the other hand, the pectin and part of hemicellulose can be dissolved, the dissolution amount of the cellulose supported by main strength is very tiny, the hollow form of the product is not damaged by the force generated by volatilization and shrinkage of colloid and the like in the subsequent drying and carbonization processes, the product is prevented from being crushed due to extrusion impact in the filling process, and the activated carbon can be recycled.
In the preparation method of the activated carbon, the cyclic bamboo charcoal carbonized material is immersed in a calcium-magnesium solution to adsorb calcium ions and magnesium ions, wherein the calcium-magnesium solution can be a solution containing calcium ions and magnesium ions at the same time or two solutions containing calcium ions and magnesium ions respectively. After the calcium ions and the magnesium ions are loaded on the annular bamboo charcoal carbonized material, the loaded calcium ions can improve the activity of the algae cell coagulin on the activated carbon, can also improve the microorganism density of the microcystis cells, and effectively improves the removal of COD in sewage by microorganisms. Magnesium ions are one of the components constituting chlorophyll and are also activators of enzymes, and an increase in the content of magnesium ions promotes algae formation into a population. The coexisting calcium and magnesium ions enhance microbial diversity and community abundance. Thus, the activated carbon adsorbs oxygen and organic matters, and the organic matters adsorbed by the micropores of the activated carbon are desorbed under the action of the external enzymes of the microorganisms through the synergistic effect of microbial degradation, so that the adsorption capacity of the micropores is recovered.
In a word, the preparation method of the activated carbon fully utilizes the natural characteristics of the square bamboo to prepare the activated carbon capable of reducing the COD of sewage, and simultaneously adopts a series of technical means to inhibit the defects of the square bamboo and further improve the sewage treatment advantages of the activated carbon.
Optionally, the inner diameter of the square bamboo tube is 8-10mm, and the outer diameter is 16-25mm. Optionally, the length of the bamboo ring is 2-4cm.
Optionally, the soaking the bamboo rings in the hydrochloric acid solution comprises: the bamboo rings are placed in hydrochloric acid solution with the concentration of 10-30wt% for soaking for 0.5-5 hours. The hydrochloric acid solution concentration is preferably 10-20wt%. Preferably, the soaking time is 1.5-3 hours, for example, 2 hours, 2.5 hours, etc.
Optionally, the clean water washing comprises washing the bamboo loops with tap water until the pH is near 7. Optionally, the drying comprises drying by using a drying box, and weighing the dried bamboo rings for a plurality of times in the drying process until the bamboo rings are constant in quality.
Optionally, the carbonization treatment comprises the steps of putting the dried bamboo rings into a box-type atmosphere protection furnace, gradually heating to 400-800 ℃ under the protection of nitrogen, and preserving heat for 1-2 hours.
Optionally, the immersing the cyclic bamboo charcoal carbonized material in a calcium-magnesium solution to adsorb calcium ions and magnesium ions includes: according to the mass ratio of the calcium-magnesium solution to the annular bamboo charcoal carbonized material of 2:1, placing the annular bamboo charcoal carbonized material into a mixture of CaCl with the concentration of 5-10wt% 2 Solution and MgCl with concentration of 2-5wt% 2 And (3) immersing the calcium-magnesium solution formed by mixing the solutions for 2-24 hours, and then drying the annular bamboo charcoal carbonized material to obtain the annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions. The impregnation time is preferably 8 to 15 hours, for example, 10 hours, 11 hours, 12 hours, 13 hours, etc.
Alternatively, the activation treatment process uses only CO 2 The gas acts as an activating gas. For small-molecule, less polar organic pollutants, micropores play a decisive role in adsorption; the specific surface area and pore volume of mesopores play an important role for organic matters with molecular weights of 6-9 kDa; for organic matter (humic acid) with molecular weight between 10 and 20kDa, the specific surface area of the mesopores plays a decisive role. By CO 2 The micropore volume and the mesopore volume of the activated carbon can be obviously improved after activation.
Optionally, the activation treatment comprises placing the annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions into a box-type atmosphere protection furnace, and continuously introducing CO 2 Gradually heating to 600-800 ℃ under the gas condition and preserving heat for 1-2h, wherein CO 2 The gas flow is controlled to be 0.1-0.5L/min.
According to a second aspect of the present application, there is provided a process for the preparation of activated carbon as described in the first aspect above.
After the square bamboo is used as renewable resources to prepare the active carbon, the natural annular structure, namely the natural molding, can be maintained, and the mechanical molding cost of the active carbon is reduced. Due to the annular hollow structure of the activated carbon, the water flow resistance and the equipment energy consumption can be reduced. The method does not use the steps of forming the binder such as coal tar and the like in the preparation process of the activated carbon, is environment-friendly in the preparation process, has low cost and is suitable for industrial production. The activated carbon prepared from square bamboo has developed microscopic medium-large pore structure, and provides biological flora living and accumulating space and growth nutrients after calcium and magnesium ions are modified, so that macromolecular organic pollutants in sewage are effectively treated in a synergistic way. In addition, the activated carbon is easy to regenerate after sewage COD is treated, and the adsorption capacity of the activated carbon can be recovered after calcination.
The application is further described below with reference to the drawings and detailed description. Additional aspects and advantages of the application 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 application.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments and, together with the description, serve to explain the principles of the application. In the drawings:
FIG. 1 is a schematic flow chart of a method for preparing activated carbon according to an embodiment of the present application.
FIG. 2 is a graph showing the adsorption and desorption curves of nitrogen in the activated carbon obtained in Experimental example 6.
FIG. 3 is a graph showing pore size distribution of the activated carbon obtained in Experimental example 6.
Fig. 4 is an SEM image of the activated carbon obtained in experimental example 3.
Fig. 5 is an SEM image of the activated carbon obtained in experimental example 6.
Detailed Description
The following is a clear and complete description of embodiments of the present application with reference to the accompanying drawings. Those of ordinary skill in the art will be able to implement the application based on these descriptions. Before describing the embodiments of the present disclosure with reference to the drawings, it should be noted in particular that:
the technical solutions and technical features provided in the respective sections including the following description in the present application may be combined with each other without collision.
The matters set forth in the following description generally relate to only some, but not all, of the embodiments of the present disclosure and, therefore, all other embodiments that may be made by one of ordinary skill in the art without the benefit of the present disclosure are to be considered within the scope of the present disclosure.
FIG. 1 is a schematic flow chart of a method for preparing activated carbon according to an embodiment of the present application. As shown in fig. 1, the method includes:
step S100: taking bamboo tubes as raw materials, and cutting the bamboo tubes into bamboo rings with required lengths. The square bamboo tube can be obtained from 1-1.5 years old square bamboo, so as to control the inner diameter of square bamboo to 8-10mm and the outer diameter to 16-25mm. In addition, the length of the bamboo ring can be controlled to be 2-4cm when the bamboo ring is cut off. The cutting mode can adopt various cutting modes, but the cutting surface is preferably kept flat; the cut-off surface can be the cross section of a square bamboo tube so that the bamboo ring is in a more regular annular structure. The relevant size parameters are mainly obtained based on the inventor according to the natural growth condition of square bamboo and combined with the technical experience of activated carbon preparation and the technical experience of sewage treatment. If square bamboo with longer growth period is selected as a raw material, the inner and outer diameters of the square bamboo tube are larger, and finally the contact area of the activated carbon and sewage on the whole can be influenced; if square bamboo with shorter growth period is selected as raw material, the square bamboo is not mature enough to fully form and maintain the hollow annular structure of the activated carbon. In addition, the square bamboo which is 1-1.5 years old is selected to be matched with the growth and cultivation period of the square bamboo, so that the industrialized production of the activated carbon is facilitated.
Step S200: soaking the bamboo rings in hydrochloric acid solution, cleaning with clear water, and drying. The method can remove indissoluble inorganic matters in and on the surface of the square bamboo on one hand, reduce the influence of external factors on the performance of the activated carbon, dissolve the pectin and part of hemicellulose on the other hand, and the cellulose supported by the main strength is very tiny in the dissolution amount of hydrochloric acid, so that the hollow form of the product is not damaged by the force generated by volatilization and shrinkage of colloid and the like in the subsequent drying and carbonization processes, the product is prevented from being crushed due to extrusion impact in the filling process, and the activated carbon can be recycled.
The soaking the bamboo rings in the hydrochloric acid solution specifically comprises the following steps: the bamboo rings are placed in hydrochloric acid solution with the concentration of 10-30wt% for soaking for 0.5-5 hours. The hydrochloric acid solution concentration is preferably 10-20wt%. Preferably, the soaking time is 1.5-3 hours, for example, 2 hours, 2.5 hours, etc. In addition, in implementation, the bamboo rings can be placed in the hydrochloric acid solution according to the ratio of the mass of the hydrochloric acid solution to the mass of the bamboo rings of 5:1.
After soaking, the bamboo rings can be fished out, and then the bamboo rings are washed by tap water until the pH value is close to 7. The drying can comprise drying by using a drying box, and weighing the dried bamboo rings for a plurality of times in the drying process until the bamboo rings are constant in quality, so that the drying speed is high, and the bamboo rings can be sufficiently high in dryness.
Step S300: and (3) carbonizing the dried bamboo rings to obtain the annular bamboo charcoal carbonized material with the shape of the bamboo rings. Carbonization is a conventional process in the preparation of activated carbon. The carbonization treatment can specifically comprise the steps of putting the dried bamboo rings into a box-type atmosphere protection furnace, gradually heating to 400-800 ℃ under the protection of nitrogen, and preserving heat for 1-2 hours, so as to obtain the annular bamboo charcoal carbonized material with the annular shape of the bamboo.
Step S400: and immersing the annular bamboo charcoal carbonized material in a calcium-magnesium solution so as to adsorb calcium ions and magnesium ions. The calcium-magnesium solution may be either one solution containing both calcium and magnesium ions or two solutions containing both calcium ions and magnesium ions. After the calcium ions and the magnesium ions are loaded on the annular bamboo charcoal carbonized material, the loaded calcium ions can improve the activity of the algae cell coagulin on the activated carbon, can also improve the microorganism density of the microcystis cells, and effectively improves the removal of COD in sewage by microorganisms. Magnesium ions are one of the components constituting chlorophyll and are also activators of enzymes, and an increase in the content of magnesium ions promotes algae formation into a population. The coexisting calcium and magnesium ions enhance microbial diversity and community abundance. Thus, the activated carbon adsorbs oxygen and organic matters, and the organic matters adsorbed by the micropores of the activated carbon are desorbed under the action of the external enzymes of the microorganisms through the synergistic effect of microbial degradation, so that the adsorption capacity of the micropores is recovered.
Optionally, the immersing the cyclic bamboo charcoal carbonized material in a calcium-magnesium solution to adsorb calcium ions and magnesium ions includes: according to the mass ratio of the calcium-magnesium solution to the annular bamboo charcoal carbonized material of 2:1, placing the annular bamboo charcoal carbonized material into a mixture of CaCl with the concentration of 5-10wt% 2 Solution and MgCl with concentration of 2-5wt% 2 And (3) immersing the calcium-magnesium solution formed by mixing the solutions for 2-24 hours, and then drying the annular bamboo charcoal carbonized material to obtain the annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions. The impregnation time is preferably 8 to 15 hours, for example, 10 hours, 11 hours, 12 hours, 13 hours, etc.
Step S500: and (3) activating the annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions to obtain an active carbon product.
Alternatively, the activation treatment process uses only CO 2 The gas acts as an activating gas. For small-molecule, less polar organic pollutants, micropores play a decisive role in adsorption; the specific surface area and pore volume of mesopores play an important role for organic matters with molecular weights of 6-9 kDa; for organic matter (humic acid) with molecular weight between 10 and 20kDa, the specific surface area of the mesopores plays a decisive role. By CO 2 The micropore volume and the mesopore volume of the activated carbon can be obviously improved after activation.
Optionally, the activation treatment comprises placing the annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions into a box-type atmosphere protection furnace, and continuously introducing CO 2 Gradually heating to 600-800 ℃ under the gas condition and preserving heat for 1-2h, wherein CO 2 The gas flow is controlled to be 0.1-0.5L/min.
Experimental example 1
According to the method for producing activated carbon of the above example, the production of activated carbon is divided into the following steps (parts referred to in the following are parts by weight, unless otherwise specified):
cutting: and selecting a square bamboo tube part with 1 year of bamboo age, cutting to 2-4cm length, and keeping the cut end face flat.
Acid soaking: 10 parts of the cut bamboo rings are weighed and put into 50 parts of 20wt% hydrochloric acid for soaking for 2 hours.
Washing: washing the acid-soaked bamboo rings with clear water for multiple times until the bamboo rings are neutral, namely finishing washing.
And (3) drying: and (3) placing the washed bamboo rings into a constant-temperature drying oven, keeping the temperature at 50 ℃ for 12 hours, keeping the temperature at 80 ℃ for 12 hours, weighing the bamboo rings for one time at intervals of 2 hours, and finishing drying after the constant quality.
Carbonizing treatment: and (3) putting the dried bamboo rings into a box-type atmosphere protection furnace, setting the heating rate to be 3 ℃/min, heating to 650 ℃, and preserving heat for 1.5h.
Dipping: weigh 5 parts CaCl 2 And 2 parts of MgCl 2 A calcium-magnesium solution was prepared by dissolving in 100 parts of water. 10 parts of annular bamboo charcoal carbonized material is weighed and put into a prepared calcium-magnesium solution, immersed for 12 hours, and then put into a constant temperature drying oven for drying at 80 ℃ for 12 hours.
Calcination (activation treatment): placing the dried annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions into a box-type atmosphere protection furnace, setting the heating rate to be 5 ℃/min to 600 ℃, and setting CO to be equal to the heating rate 2 The flow is 0.2L/min, and the activated carbon product is obtained after the constant temperature is maintained for 1 h.
Experimental example 2
According to the method for producing activated carbon of the above example, the production of activated carbon is divided into the following steps (parts referred to in the following are parts by weight, unless otherwise specified):
cutting: and selecting a square bamboo tube part with 1 year of bamboo age, cutting to 2-4cm length, and keeping the cut end face flat.
Acid soaking: 10 parts of the cut bamboo rings are weighed and put into 50 parts of 20wt% hydrochloric acid for soaking for 2 hours.
Washing: washing the acid-soaked bamboo rings with clear water for multiple times until the bamboo rings are neutral, namely finishing washing.
And (3) drying: and (3) placing the washed bamboo rings into a constant-temperature drying oven, keeping the temperature at 50 ℃ for 12 hours, keeping the temperature at 80 ℃ for 12 hours, weighing the bamboo rings for one time at intervals of 2 hours, and finishing drying after the constant quality.
Carbonizing treatment: and (3) putting the dried bamboo rings into a box-type atmosphere protection furnace, setting the heating rate to be 3 ℃/min, heating to 650 ℃, and preserving heat for 1.5h.
Dipping: 10 parts of CaCl were weighed out 2 And 2 parts of MgCl 2 A calcium-magnesium solution was prepared by dissolving in 100 parts of water. 10 parts of annular bamboo charcoal carbonized material is weighed and put into a prepared calcium-magnesium solution, immersed for 12 hours, and then put into a constant temperature drying oven for drying at 80 ℃ for 12 hours.
Calcination (activation treatment): placing the dried annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions into a box-type atmosphere protection furnace, setting the heating rate to be 5 ℃/min to 600 ℃, and setting CO to be equal to the heating rate 2 The flow is 0.2L/min, and the activated carbon product is obtained after the constant temperature is maintained for 1 h.
Experimental example 3
According to the method for producing activated carbon of the above example, the production of activated carbon is divided into the following steps (parts referred to in the following are parts by weight, unless otherwise specified):
cutting: and selecting a square bamboo tube part with 1 year of bamboo age, cutting to 2-4cm length, and keeping the cut end face flat.
Acid soaking: 10 parts of the cut bamboo rings are weighed and put into 50 parts of 20wt% hydrochloric acid for soaking for 2 hours.
Washing: washing the acid-soaked bamboo rings with clear water for multiple times until the bamboo rings are neutral, namely finishing washing.
And (3) drying: and (3) placing the washed bamboo rings into a constant-temperature drying oven, keeping the temperature at 50 ℃ for 12 hours, keeping the temperature at 80 ℃ for 12 hours, weighing the bamboo rings for one time at intervals of 2 hours, and finishing drying after the constant quality.
Carbonizing treatment: and (3) putting the dried bamboo rings into a box-type atmosphere protection furnace, setting the heating rate to be 3 ℃/min, heating to 650 ℃, and preserving heat for 1.5h.
Dipping: 10 parts of CaCl were weighed out 2 And 5 parts of MgCl 2 A calcium-magnesium solution was prepared by dissolving in 100 parts of water. 10 parts of annular bamboo charcoal carbonized material is weighed and put into a prepared calcium-magnesium solution, immersed for 12 hours, and then put into a constant temperature drying oven for drying at 80 ℃ for 12 hours.
Calcination (activation treatment): placing the dried annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions into a box-type atmosphere protection furnace, setting the heating rate to be 5 ℃/min to 600 ℃, and setting CO to be equal to the heating rate 2 The flow is 0.2L/min, and the activated carbon product is obtained after the constant temperature is maintained for 1 h.
Experimental example 4
According to the method for producing activated carbon of the above example, the production of activated carbon is divided into the following steps (parts referred to in the following are parts by weight, unless otherwise specified):
cutting: and selecting a square bamboo tube part with 1 year of bamboo age, cutting to 2-4cm length, and keeping the cut end face flat.
Acid soaking: 10 parts of the cut bamboo rings are weighed and put into 50 parts of 20wt% hydrochloric acid for soaking for 2 hours.
Washing: washing the acid-soaked bamboo rings with clear water for multiple times until the bamboo rings are neutral, namely finishing washing.
And (3) drying: and (3) placing the washed bamboo rings into a constant-temperature drying oven, keeping the temperature at 50 ℃ for 12 hours, keeping the temperature at 80 ℃ for 12 hours, weighing the bamboo rings for one time at intervals of 2 hours, and finishing drying after the constant quality.
Carbonizing treatment: and (3) putting the dried bamboo rings into a box-type atmosphere protection furnace, setting the heating rate to be 3 ℃/min, heating to 650 ℃, and preserving heat for 1.5h.
Dipping: 10 parts of CaCl were weighed out 2 And 5 parts of MgCl 2 A calcium-magnesium solution was prepared by dissolving in 100 parts of water. 10 parts of annular bamboo charcoal carbonized material is weighed and put into a prepared calcium-magnesium solution, immersed for 12 hours, and then put into a constant temperature drying oven for drying at 80 ℃ for 12 hours.
Calcination (activation treatment): placing the dried annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions into a box-type atmosphere protection furnace, setting the heating rate to be 5 ℃/min to 700 ℃, and setting CO 2 The flow is 0.2L/min, and the activated carbon product is obtained after the constant temperature is maintained for 1 h.
Experimental example 5
According to the method for producing activated carbon of the above example, the production of activated carbon is divided into the following steps (parts referred to in the following are parts by weight, unless otherwise specified):
cutting: and selecting a square bamboo tube part with 1 year of bamboo age, cutting to 2-4cm length, and keeping the cut end face flat.
Acid soaking: 10 parts of the cut bamboo rings are weighed and put into 50 parts of 20wt% hydrochloric acid for soaking for 2 hours.
Washing: washing the acid-soaked bamboo rings with clear water for multiple times until the bamboo rings are neutral, namely finishing washing.
And (3) drying: and (3) placing the washed bamboo rings into a constant-temperature drying oven, keeping the temperature at 50 ℃ for 12 hours, keeping the temperature at 80 ℃ for 12 hours, weighing the bamboo rings for one time at intervals of 2 hours, and finishing drying after the constant quality.
Carbonizing treatment: and (3) putting the dried bamboo rings into a box-type atmosphere protection furnace, setting the heating rate to be 3 ℃/min, heating to 650 ℃, and preserving heat for 1.5h.
Dipping: 10 parts of CaCl were weighed out 2 And 5 parts of MgCl 2 A calcium-magnesium solution was prepared by dissolving in 100 parts of water. 10 parts of annular bamboo charcoal carbonized material is weighed and put into a prepared calcium-magnesium solution, immersed for 12 hours, and then put into a constant temperature drying oven for drying at 80 ℃ for 12 hours.
Calcination (activation treatment): placing the dried annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions into a box-type atmosphere protection furnace, setting the heating rate to 5 ℃/min to 800 ℃, and setting CO 2 The flow is 0.2L/min, and the activated carbon product is obtained after the constant temperature is maintained for 1 h.
Experimental example 6
According to the method for producing activated carbon of the above example, the production of activated carbon is divided into the following steps (parts referred to in the following are parts by weight, unless otherwise specified):
cutting: and selecting a square bamboo tube part with 1 year of bamboo age, cutting to 2-4cm length, and keeping the cut end face flat.
Acid soaking: 10 parts of the cut bamboo rings are weighed and put into 50 parts of 20wt% hydrochloric acid for soaking for 2 hours.
Washing: washing the acid-soaked bamboo rings with clear water for multiple times until the bamboo rings are neutral, namely finishing washing.
And (3) drying: and (3) placing the washed bamboo rings into a constant-temperature drying oven, keeping the temperature at 50 ℃ for 12 hours, keeping the temperature at 80 ℃ for 12 hours, weighing the bamboo rings for one time at intervals of 2 hours, and finishing drying after the constant quality.
Carbonizing treatment: and (3) putting the dried bamboo rings into a box-type atmosphere protection furnace, setting the heating rate to be 3 ℃/min, heating to 650 ℃, and preserving heat for 1.5h.
Dipping: 10 parts of CaCl were weighed out 2 And 5 parts of MgCl 2 A calcium-magnesium solution was prepared by dissolving in 100 parts of water. Weighing 10 parts of annular bamboo charcoal carbonized material and putting the material into a prepared calcium-magnesium solutionSoaking for 12h, and then placing into a constant temperature drying oven to be dried for 12h at 80 ℃.
Calcination (activation treatment): placing the dried annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions into a box-type atmosphere protection furnace, setting the heating rate to 5 ℃/min to 800 ℃, and setting CO 2 The flow is 0.2L/min, and the activated carbon product is obtained after constant temperature is maintained for 2 hours.
Experimental results
I. The activated carbon of experimental examples 1-6 was used for static sewage treatment for 1h, and the COD index of the sewage before treatment and the COD index of the sewage after treatment were measured, respectively, to obtain COD removal rates. COD removal rate= (pretreatment sewage COD index-post-treatment sewage COD index)/pretreatment sewage COD index. The results are shown in Table 1.
TABLE 1
The results show that the COD removal rate of the activated carbon of the experimental examples 1-6 in static sewage treatment for 1h is at least 40.38% and at most 44.21%.
And II, performing static sewage treatment of different static adsorption time by using the activated carbon in the experimental examples 1-2, and respectively measuring the COD index of the sewage before treatment and the COD index of the sewage after treatment in each static adsorption time to obtain the COD removal rate in each static adsorption time. COD removal rate = (pretreatment sewage COD index-pretreatment sewage COD index for each static adsorption time)/pretreatment sewage COD index for each static adsorption time. The results are shown in Table 2.
TABLE 2
The results show that the content of calcium and magnesium ions is increased, the synergistic effect of microorganisms is improved, namely, after the adsorption time is prolonged, the removal rate of COD by the activated carbon is obviously improved.
III, FIG. 2 is a graph showing the adsorption and desorption curves of nitrogen in the activated carbon obtained in Experimental example 6. FIG. 3 is a graph showing pore size distribution of the activated carbon obtained in Experimental example 6. Fig. 4 is an SEM image of the activated carbon obtained in experimental example 3. Fig. 5 is an SEM image of the activated carbon obtained in experimental example 6. As shown in FIG. 2, the nitrogen adsorption and desorption curve of experimental example 6 is a type I isotherm, and the specific surface area of the sample of experimental example 6 is 973.093m2/g. From the pore size distribution diagram of FIG. 3, the pore size of the micropores is mainly 3-5nm, and the activated carbon has a developed mesopore structure and good adsorption effect on most of sewage organic matters. As can be seen from fig. 4 and fig. 5, the activated carbon has a regular structure, and when the activation temperature is low, the activated carbon mainly has macropores, has a better adsorption capacity on macromolecular organic matters, and when the activation temperature is increased, the activated carbon mainly has small pores, and the pores are more uniform, so that the square bamboo has higher strength due to the regular structure.
The content of the present application is described above. Those of ordinary skill in the art will be able to implement the application based on these descriptions. Based on the foregoing, it should be appreciated that all other embodiments, which may be obtained by persons skilled in the art without undue burden, are within the scope of the present application.
Claims (10)
1. The preparation method of the activated carbon for removing the COD in the sewage is characterized by comprising the following steps:
taking bamboo tubes as raw materials, and cutting the bamboo tubes into bamboo rings with required lengths;
soaking the bamboo rings in hydrochloric acid solution, cleaning with clear water, and drying;
carbonizing the dried bamboo rings to obtain annular bamboo charcoal carbonized materials with the shape of the bamboo rings;
immersing the annular bamboo charcoal carbonized material in a calcium-magnesium solution so as to adsorb calcium ions and magnesium ions;
activating the annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions to obtain an active carbon product;
the inner diameter of the square bamboo tube is 8-10mm, the outer diameter is 16-25mm, and the length of the bamboo ring is 2-4cm;
immersing the annular bamboo charcoal carbonized material in a calcium-magnesium solution to adsorb calcium ions and magnesium ions comprises: according to the mass of calcium-magnesium solution and the cyclic bambooCarbon carbonized material mass ratio 2:1, placing the annular bamboo charcoal carbonized material into a mixture of CaCl with the concentration of 5-10wt% 2 Solution and MgCl with concentration of 2-5wt% 2 And (3) immersing the calcium-magnesium solution formed by mixing the solutions for 2-24 hours, and then drying the annular bamboo charcoal carbonized material to obtain the annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions.
2. The method of claim 1, wherein: the bamboo rings are soaked in hydrochloric acid solution, which comprises the following steps: the bamboo rings are placed in hydrochloric acid solution with the concentration of 10-30wt% for soaking for 0.5-5 hours.
3. The method of claim 2, wherein: the bamboo rings are soaked in hydrochloric acid solution, which comprises the following steps: the bamboo rings are placed in hydrochloric acid solution with the concentration of 10-20wt% for soaking time of 1.5-3 hours.
4. The method of claim 1, wherein: the clean water washing comprises the step of washing the bamboo rings by using tap water until the pH value is close to 7.
5. The method of claim 1, wherein: the drying comprises the steps of drying by using a drying box, and weighing the dried bamboo rings for a plurality of times in the drying process until the bamboo rings are constant in quality.
6. The method of claim 1, wherein: the carbonization treatment comprises the steps of putting the dried bamboo rings into a box-type atmosphere protection furnace, gradually heating to 400-800 ℃ under the protection of nitrogen, and preserving heat for 1-2 hours.
7. The method of claim 1, wherein: the soaking time is 8-15 hours.
8. The method of claim 1, wherein: the activation treatment process uses only CO 2 The gas acts as an activating gas.
9. The method as recited in claim 8, wherein: the activation treatment comprises placing annular bamboo charcoal carbonized material loaded with calcium ions and magnesium ions into a box-type atmosphere protection furnace, and continuously introducing CO 2 Gradually heating to 600-800 ℃ under the gas condition and preserving heat for 1-2h, wherein CO 2 The gas flow is controlled to be 0.1-0.5L/min.
10. An activated carbon for removing sewage COD, which is characterized in that: which is obtainable by a process according to any one of claims 1 to 9.
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