CN117142471A - Modified activated carbon based on traditional Chinese medicine waste residues and preparation method thereof - Google Patents
Modified activated carbon based on traditional Chinese medicine waste residues and preparation method thereof Download PDFInfo
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- CN117142471A CN117142471A CN202311436510.9A CN202311436510A CN117142471A CN 117142471 A CN117142471 A CN 117142471A CN 202311436510 A CN202311436510 A CN 202311436510A CN 117142471 A CN117142471 A CN 117142471A
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- traditional chinese
- chinese medicine
- activated carbon
- modified activated
- waste residue
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000002699 waste material Substances 0.000 title claims abstract description 62
- 239000003814 drug Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 32
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 239000011787 zinc oxide Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000011592 zinc chloride Substances 0.000 claims abstract description 11
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- 238000004108 freeze drying Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 12
- 239000002243 precursor Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 4
- 239000005539 carbonized material Substances 0.000 description 4
- 239000011630 iodine Substances 0.000 description 4
- 229910052740 iodine Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 229940126680 traditional chinese medicines Drugs 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 235000009917 Crataegus X brevipes Nutrition 0.000 description 1
- 235000013204 Crataegus X haemacarpa Nutrition 0.000 description 1
- 235000009685 Crataegus X maligna Nutrition 0.000 description 1
- 235000009444 Crataegus X rubrocarnea Nutrition 0.000 description 1
- 235000009486 Crataegus bullatus Nutrition 0.000 description 1
- 235000017181 Crataegus chrysocarpa Nutrition 0.000 description 1
- 235000009682 Crataegus limnophila Nutrition 0.000 description 1
- 235000004423 Crataegus monogyna Nutrition 0.000 description 1
- 240000000171 Crataegus monogyna Species 0.000 description 1
- 235000002313 Crataegus paludosa Nutrition 0.000 description 1
- 235000009840 Crataegus x incaedua Nutrition 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 244000303040 Glycyrrhiza glabra Species 0.000 description 1
- 235000006200 Glycyrrhiza glabra Nutrition 0.000 description 1
- 240000004153 Hibiscus sabdariffa Species 0.000 description 1
- 235000001018 Hibiscus sabdariffa Nutrition 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 235000011477 liquorice Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 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
- 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
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to the technical field of active carbon preparation, and relates to a modified active carbon based on traditional Chinese medicine waste residues and a preparation method thereof. The preparation method comprises the following steps: crushing the traditional Chinese medicine waste residue to 500-600 meshes, mixing the traditional Chinese medicine waste residue, tetrapod-like zinc oxide and zinc chloride solution, performing ultrasonic treatment for 2-6 hours, performing freeze drying, crushing to 200-300 meshes, and performing sectional heat treatment, wherein the sectional heat treatment is performed for 60-80 minutes at 600-650 ℃, 30 minutes at 700-720 ℃ and 60-80 minutes at 600-650 ℃. The preparation method is a method for recycling traditional Chinese medicine waste residues, and the obtained modified activated carbon has excellent adsorption performance.
Description
Technical Field
The invention belongs to the technical field of active carbon preparation, and relates to a modified active carbon based on traditional Chinese medicine waste residues and a preparation method thereof.
Background
The Chinese medicine is prepared with plant, animal and mineral material in 87%. The output of a large amount of traditional Chinese medicinal materials brings about a large amount of traditional Chinese medicinal waste residues, and the traditional Chinese medicinal waste residues are generally wet materials, have high water content, are easy to be decomposed and deteriorated, emit malodor and grow bacteria. The traditional Chinese medicine waste residue treatment form mainly comprises fixed area stacking, landfill, incineration and the like, which not only costs a great deal of funds and occupies a great deal of land, but also causes the waste of resources and secondary pollution of water and atmosphere to a certain extent. Therefore, a resource utilization method of the traditional Chinese medicine waste residue is required to be sought.
CN105731455a discloses a method for preparing active carbon from Chinese medicinal residues, which comprises the steps of carrying out pretreatment on the Chinese medicinal residues in a carbonization furnaceCarbonization by dry distillation, and further using 50wt% H 3 PO 4 Activating the solution and performing ultrasonic treatment; then placing the mixture into an activation furnace, activating the mixture by using steam at high temperature, grinding the carbonized material, washing the carbonized material with water, drying the carbonized material, and sieving the carbonized material in a grading manner to obtain the activated carbon. The method adopts the zinc chloride method to prepare the active carbon by single Chinese medicinal materials, does not improve the process of the active carbon, and is not suitable for recycling the Chinese medicinal waste residues after compounding of multiple medicinal materials.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a preparation method of modified activated carbon based on traditional Chinese medicine waste residues, which is further improved to obtain better gaps between activated carbon layers, obtain activated carbon with better technical parameters and is suitable for compounding various traditional Chinese medicinal materials.
Based on the above objects, the present invention provides a modified activated carbon based on waste residues of traditional Chinese medicines and a preparation method thereof to meet the needs in the art.
In one aspect, the invention relates to a method for preparing modified activated carbon based on traditional Chinese medicine waste residues, which comprises the following steps: crushing the traditional Chinese medicine waste residue to 500-600 meshes, mixing the traditional Chinese medicine waste residue, tetrapod-like zinc oxide and zinc chloride solution, performing ultrasonic treatment for 2-6 hours, performing freeze drying, crushing to 200-300 meshes, and performing sectional heat treatment, wherein the sectional heat treatment is performed for 60-80 minutes at 600-650 ℃, 30 minutes at 700-720 ℃ and 60-80 minutes at 600-650 ℃.
In the preparation method of the modified activated carbon based on the traditional Chinese medicine waste residue, each 10g of the traditional Chinese medicine waste residue corresponds to 0.5-1 g of tetrapod-like zinc oxide and 10-15 mL of 15wt% zinc chloride solution.
Further, in the preparation method of the modified activated carbon based on the traditional Chinese medicine waste residue, the diameter of the tetrapod-like zinc oxide is 100-300 nm.
Further, in the preparation method of the modified activated carbon based on the traditional Chinese medicine waste residue, the heating rate of the sectional heat treatment is 10 ℃/min.
Further, in the preparation method of the modified activated carbon based on the traditional Chinese medicine waste residue, the sectional heat treatment is carried out for 80min at 600 ℃, 30min at 700 ℃ and 80min at 600 ℃.
Further, in the preparation method of the modified activated carbon based on the traditional Chinese medicine waste residue, the sectional heat treatment is carried out at 650 ℃ for 60min,720 ℃ for 30min and 650 ℃ for 60min.
On the other hand, the invention relates to a modified activated carbon based on traditional Chinese medicine waste residues, which is prepared by adopting the preparation method of the modified activated carbon based on traditional Chinese medicine waste residues.
Through the technical scheme, the technical scheme provided by the invention has at least the following beneficial effects or advantages:
the invention provides a preparation method of modified activated carbon based on traditional Chinese medicine waste residue, which is characterized in that the traditional Chinese medicine waste residue is crushed by superfine crushing and is matched with tetrapod-like zinc oxide, so that the adsorptivity of the prepared modified activated carbon is greatly improved. The method adopts a sectional heat treatment mode, utilizes short-time high-temperature treatment to ensure that the tetrapod-like zinc oxide is combined with the material more fully, improves the diffusion rate and concentration of zinc in the modified activated carbon, further improves the original zinc chloride method, and further improves the adsorptivity of the obtained modified activated carbon.
Detailed Description
In order that those skilled in the art will better understand the technical solution of the present invention, the present invention will be further described with reference to specific examples, but the examples are not intended to limit the present invention.
The experimental methods and the detection methods described in the following examples are all conventional methods unless otherwise specified; the test articles and the raw materials are available on the market unless otherwise specified.
Example 1
The embodiment provides a preparation process of modified activated carbon based on traditional Chinese medicine waste residues.
Waste residues of traditional Chinese medicines: soaking 25g of dark plum, 6g of dried orange peel, 8g of roselle, 12g of hawthorn, 8g of mulberry, 3g of liquorice and 120g of rock candy in 1800mL of clear water for 30min, boiling with big fire, boiling with small fire for 30min, filtering, and drying in a hot oven at 80 ℃ for 24h to obtain the traditional Chinese medicine waste residue.
S1: crushing the traditional Chinese medicine waste residue to 500 meshes by adopting an ultrafine grinder (WFJ-15), mixing 10g of the traditional Chinese medicine waste residue, 0.5g of tetrapod-like zinc oxide (purchased from Oncorhynchi novel carbon material Changzhou Co., ltd., diameter of 100-300 nm) and 10mL of 15wt% zinc chloride solution, performing ultrasonic treatment for 2 hours, performing quick freeze drying, and crushing to 200 meshes to obtain the modified activated carbon precursor.
S2: adding the modified activated carbon precursor into a crucible, heating to 600 ℃ in a muffle furnace at a speed of 10 ℃/min for 80min, heating to 700 ℃ for 30min, heating to 600 ℃ for 80min, taking out the modified activated carbon material after normal cooling to room temperature, and storing in a dryer for standby.
Example 2
The embodiment provides a preparation process of modified activated carbon based on traditional Chinese medicine waste residues.
The sources of the test materials were the same as in example 1.
S1: the traditional Chinese medicine waste residue is crushed to 600 meshes by an ultrafine grinder, 10g of traditional Chinese medicine waste residue, 0.8g of tetrapod-like zinc oxide and 12mL of 15wt% zinc chloride solution are mixed and then are subjected to ultrasonic treatment for 4 hours, and after quick freeze drying, the mixture is crushed to 300 meshes to obtain the modified activated carbon precursor.
S2: adding the modified activated carbon precursor into a crucible, heating to 650 ℃ at a speed of 10 ℃/min in a muffle furnace, treating for 60min, treating for 30min at 720 ℃ and treating for 60min at 650 ℃, taking out the modified activated carbon material after the modified activated carbon material is normally cooled to room temperature, and storing in a dryer for standby.
Example 3
The embodiment provides a preparation process of modified activated carbon based on traditional Chinese medicine waste residues.
The sources of the test materials were the same as in example 1.
S1: the traditional Chinese medicine waste residue is crushed to 600 meshes by an ultrafine grinder, 10g of traditional Chinese medicine waste residue, 1.0g of tetrapod-like zinc oxide and 15mL of 15wt% zinc chloride solution are mixed and then are subjected to ultrasonic treatment for 6 hours, and after quick freeze drying, the mixture is crushed to 300 meshes to obtain the modified activated carbon precursor.
S2: adding the modified activated carbon precursor into a crucible, heating to 650 ℃ at a speed of 10 ℃/min in a muffle furnace, treating for 80min, treating for 30min at 700 ℃ and treating for 80min at 600 ℃, taking out the modified activated carbon material after the modified activated carbon material is normally cooled to room temperature, and storing in a dryer for standby.
Example 4
The embodiment provides a preparation process of modified activated carbon based on traditional Chinese medicine waste residues.
The sources of the test materials were the same as in example 1.
S1: the traditional Chinese medicine waste residue is crushed to 600 meshes by an ultrafine grinder, 10g of traditional Chinese medicine waste residue, 0.8g of tetrapod-like zinc oxide and 12mL of 15wt% zinc chloride solution are mixed and then are subjected to ultrasonic treatment for 4 hours, and after quick freeze drying, the mixture is crushed to 300 meshes to obtain the modified activated carbon precursor.
S2: adding the modified activated carbon precursor into a crucible, heating to 600 ℃ at a speed of 10 ℃/min in a muffle furnace, treating for 60min, treating for 30min at 700 ℃ and treating for 60min at 650 ℃, taking out the modified activated carbon material after the modified activated carbon material is normally cooled to room temperature, and storing in a dryer for standby.
Comparative example 1
This comparative example provides a process for preparing modified activated carbon based on the waste residue of traditional Chinese medicine, which is the same as example 1, and the preparation method is the same as example 5 of CN105731455 a.
Comparative example 2
The comparative example provides a preparation process of modified activated carbon based on waste residues of traditional Chinese medicines, and the preparation method is the same as that of example 2, except that zinc oxide is adopted to replace tetrapod-like zinc oxide.
Comparative example 3
The comparative example provides a preparation process of modified activated carbon based on the waste residue of traditional Chinese medicine, which is similar to example 2, except that the waste residue of traditional Chinese medicine is crushed to 100 meshes.
Comparative example 4
The comparative example provides a preparation process of modified activated carbon based on traditional Chinese medicine waste residue, which is the same as that of example 2, except that the traditional Chinese medicine waste residue is crushed to 1200 meshes by a superfine crusher.
Example 5
The present examples provide adsorption performance test experiments for the modified activated carbons of examples 1 to 4 and comparative examples 1 to 4.
The modified activated carbon obtained in all examples was tested for iodine adsorption value and methylene blue adsorption value according to GB/T12496.8-1999 and GB/T12496.10-1999, and the test results are shown in Table 1.
Table 1: adsorption performance test result of modified activated carbon
As shown in Table 1, the iodine adsorption value of the modified activated carbon provided by the invention is 1104.07-1272.25 mg/g, the methylene blue adsorption value is 311.81-324.92 mg/g, and the iodine adsorption value exceeds the national primary standard of activated carbon (1000 mg/g and 135 mg/g). As is clear from comparative example 1, CN105731455a exhibits poor adsorption effect when used for the waste residue of traditional Chinese medicine compounded by a plurality of traditional Chinese medicinal materials, which may affect the pore size distribution and interlayer gap size of the modified activated carbon due to the different microstructures of the respective medicinal materials when compounded by a plurality of medicinal materials. As can be seen from comparative example 2, the addition of the tetrapod-like zinc oxide changes the microscopic morphology of the modified activated carbon, and is more suitable for the adsorption of iodine and methylene blue. As is clear from comparative examples 3 and 4, the particle size of the waste residue of the chinese medicine affects the preparation of the modified activated carbon, and when the particle size of the waste residue of the chinese medicine is too small, the adsorption space of the activated carbon becomes small.
The present invention may be better implemented as described above, and the above examples are merely illustrative of preferred embodiments of the present invention and not intended to limit the scope of the present invention, and various changes and modifications made by those skilled in the art to the technical solution of the present invention should fall within the scope of protection defined by the present invention without departing from the spirit of the design of the present invention.
Claims (6)
1. The preparation method of the modified activated carbon based on the traditional Chinese medicine waste residue is characterized by comprising the following steps: crushing the traditional Chinese medicine waste residue to 500-600 meshes, mixing the traditional Chinese medicine waste residue, tetrapod-like zinc oxide and zinc chloride solution, performing ultrasonic treatment for 2-6 hours, performing freeze drying, crushing to 200-300 meshes, and performing sectional heat treatment, wherein the sectional heat treatment is performed for 60-80 minutes at 600-650 ℃, 30 minutes at 700-720 ℃ and 60-80 minutes at 600-650 ℃;
every 10g of the traditional Chinese medicine waste residue corresponds to 0.5-1 g of tetrapod-like zinc oxide and 10-15 mL of 15wt% zinc chloride solution.
2. The method for preparing modified activated carbon based on traditional Chinese medicine waste residue according to claim 1, wherein the diameter of the tetrapod-like zinc oxide is 100-300 nm.
3. The method for preparing modified activated carbon based on waste residues of traditional Chinese medicine according to claim 1, wherein the heating rate of the sectional heat treatment is 10 ℃/min.
4. The method for preparing modified activated carbon based on waste residues of traditional Chinese medicine according to claim 1, wherein the sectional heat treatment is 600 ℃ for 80min,700 ℃ for 30min and 600 ℃ for 80min.
5. The method for preparing modified activated carbon based on waste residues of traditional Chinese medicine according to claim 1, wherein the sectional heat treatment is 650 ℃ for 60min,720 ℃ for 30min, and 650 ℃ for 60min.
6. The modified activated carbon based on the traditional Chinese medicine waste residue is characterized in that the modified activated carbon based on the traditional Chinese medicine waste residue is prepared by the preparation method of the modified activated carbon based on the traditional Chinese medicine waste residue according to any one of claims 1-5.
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| CN202311436510.9A CN117142471B (en) | 2023-11-01 | 2023-11-01 | Modified activated carbon based on traditional Chinese medicine waste residues and preparation method thereof |
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| CN117142471A true CN117142471A (en) | 2023-12-01 |
| CN117142471B CN117142471B (en) | 2023-12-22 |
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|---|---|---|---|---|
| CN105080485A (en) * | 2015-09-29 | 2015-11-25 | 江苏锦宇环境工程有限公司 | Method for preparing carbon bio-adsorbent from Chinese parasol fallen leaves |
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2023
- 2023-11-01 CN CN202311436510.9A patent/CN117142471B/en active Active
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