CN109502585B - Preparation method of magnesium-nitrogen-codoped high-specific-surface-area biomass activated carbon - Google Patents
Preparation method of magnesium-nitrogen-codoped high-specific-surface-area biomass activated carbon Download PDFInfo
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- CN109502585B CN109502585B CN201811614360.5A CN201811614360A CN109502585B CN 109502585 B CN109502585 B CN 109502585B CN 201811614360 A CN201811614360 A CN 201811614360A CN 109502585 B CN109502585 B CN 109502585B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000002028 Biomass Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 244000025254 Cannabis sativa Species 0.000 claims abstract description 38
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims abstract description 38
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims abstract description 38
- 235000009120 camo Nutrition 0.000 claims abstract description 38
- 235000005607 chanvre indien Nutrition 0.000 claims abstract description 38
- 239000011487 hemp Substances 0.000 claims abstract description 38
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 30
- SVFOMDDAWOLOME-UHFFFAOYSA-N [N].[Mg] Chemical compound [N].[Mg] SVFOMDDAWOLOME-UHFFFAOYSA-N 0.000 claims abstract description 27
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 22
- 239000011592 zinc chloride Substances 0.000 claims abstract description 15
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 12
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 238000002791 soaking Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- -1 aminopyridine compound Chemical class 0.000 claims description 8
- ICSNLGPSRYBMBD-UHFFFAOYSA-N 2-aminopyridine Chemical compound NC1=CC=CC=N1 ICSNLGPSRYBMBD-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 3
- VHNQIURBCCNWDN-UHFFFAOYSA-N pyridine-2,6-diamine Chemical compound NC1=CC=CC(N)=N1 VHNQIURBCCNWDN-UHFFFAOYSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- ZZYXNRREDYWPLN-UHFFFAOYSA-N pyridine-2,3-diamine Chemical compound NC1=CC=CN=C1N ZZYXNRREDYWPLN-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 238000007598 dipping method Methods 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 13
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 8
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001569 carbon dioxide Substances 0.000 abstract description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 4
- 239000011777 magnesium Substances 0.000 abstract description 4
- 229910052749 magnesium Inorganic materials 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 239000011165 3D composite Substances 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 150000003927 aminopyridines Chemical class 0.000 abstract description 2
- 238000005554 pickling Methods 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 238000010000 carbonizing Methods 0.000 abstract 1
- 239000007789 gas Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 238000010008 shearing Methods 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010796 biological waste Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method and application of a magnesium-nitrogen co-doped biomass activated carbon material with a high specific surface area. The active carbon has a unique macroporous-mesoporous-microporous three-dimensional composite pore structure and is characterized by being co-doped with magnesium and nitrogen. The method comprises the steps of taking biomass waste hemp core as a raw material, soaking the raw material and a mixed solution of zinc chloride and magnesium chloride for a period of time after cleaning, drying and shearing pretreatment, putting the raw material into a tubular furnace after drying, carbonizing, activating and cooling in a nitrogen atmosphere. And (3) pickling and washing the obtained product with water, soaking the product in an ethanol solution of aminopyridine for a period of time, and drying the product to obtain the magnesium-nitrogen co-doped active carbon. The activated carbon has a high specific surface area and exhibits excellent carbon dioxide gas adsorption performance.
Description
Technical Field
The invention relates to a method for preparing activated carbon by taking biomass waste as a raw material, in particular to a method for preparing magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon by taking biomass as a raw material.
Background
The activated carbon has large specific surface area and strong adsorbability, and is widely applied to various fields of chemical industry, environmental protection, food processing, metallurgy, drug refinement, military chemical protection and the like. The traditional active carbon mainly takes high-quality coal as a raw material, and has higher cost. In order to reduce the cost, save energy and protect the ecological environment, the development of the active carbon taking renewable resources as raw materials has important practical significance.
Hemp is an environmentally friendly crop with the characteristics of low cost, high yield, low nutrient demand, high land utilization rate, etc. Hemp is a major source of paper, textile and rope industries. In industrial production, hemp bast is used to produce fibers. The hemp stalk is stripped to remove bast, and the remaining wood core is hemp core. Bast fibers generally account for only about 25% by mass of the hemp stems, and a large amount of hemp core as a by-product becomes a biological waste. The hemp core is composed of 40-48% of cellulose, 18-24% of hemicellulose and 21-24% of lignin, and is a very good carbon source for producing activated carbon.
In view of the above, the method for preparing the activated carbon with the high specific surface area by using the hemp core as the raw material has important significance.
Disclosure of Invention
The invention aims to provide a preparation method of magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon. And the prepared active carbon is co-doped with magnesium and nitrogen, and has high specific surface area and good performance.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon comprises the following steps:
(1) cleaning and drying hemp core, and cutting into small sections;
(2) placing the hemp core small segments into a mixed aqueous solution of zinc chloride and magnesium chloride, fully soaking, filtering, and drying at 78-82 ℃ for 12-26 h;
(3) sintering the dried hemp core small sections at high temperature under the protection of inert gas, preserving the heat for a period of time, and then naturally cooling under the protection of inert gas to obtain carbide;
(4) pickling the carbide under vacuum and reduced pressure for 10-14h, and washing with distilled water to reach neutral pH;
(5) and (3) fully soaking the carbide obtained in the step (4) in an ethanol solution of an aminopyridine compound, and drying at 78-82 ℃ for 12-26h to obtain the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon.
In the preparation method of the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon, in the step (1), the drying temperature after cleaning is 98-102 ℃, and the hemp core is cut into small sections with the length of 1-5 cm.
In the preparation method of the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon, in the step (2), the concentration of the mixed solution of zinc chloride and magnesium chloride in the mixed aqueous solution is 20-60%.
In the preparation method of the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon, in the step (2), the mass ratio of zinc chloride to magnesium chloride in the mixed aqueous solution is 1:1-4:1, the mass ratio of zinc chloride to the impregnated hemp core is 2:1-4:1, and the impregnation time of the hemp core is 18-48 hours.
In the preparation method of the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon, in the step (3), the inert gas is nitrogen or argon.
In the preparation method of the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon, in the step (3), the high-temperature sintering and the heat preservation are carried out for a period of time; heating to 900 ℃ at the speed of 5-10 ℃/min for high-temperature sintering, and keeping the temperature for 2-5 h.
In the preparation method of the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon, in the step (4), the acid used for acid washing is one or more of dilute hydrochloric acid, dilute sulfuric acid or dilute nitric acid.
In the preparation method of the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon, in the step (5), the aminopyridine compound is more than one of 2-aminopyridine, 2, 3-diaminopyridine and 2, 6-diaminopyridine.
In the preparation method of the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon, in the step (5), the concentration of the aminopyridine compound in the ethanol solution of the aminopyridine compound is 0.2-0.5 g/ml.
In the preparation method of the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon, in the step (5), the impregnation time is 4-12 h.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention takes the hemp core as the raw material to produce the active carbon, is a method with low cost and easy processing, and simultaneously realizes the comprehensive utilization of wastes. The hemp core has a unique three-dimensional interconnected pore structure, and the active carbon taking the hemp core as a raw material has a unique macroporous-mesoporous-microporous three-dimensional composite pore structure, and is not only a high-efficiency adsorbent, but also a good heteroatom carrier.
2. According to the magnesium-nitrogen co-doped active carbon taking the hemp core as the raw material, magnesium oxide and aminopyridine are introduced in the carbonization and activation process of the hemp core, and co-doping of magnesium and nitrogen on the active carbon plays a synergistic role, so that the adsorption capacity of the active carbon on carbon dioxide is improved. The method has wide application in drainage areas such as capacitors, electrode materials and the like, and is not limited to the adsorption field of the invention. And then introducing nitrogen elements on the surface of the formed activated carbon. The obtained activated carbon has large specific surface area, and the co-doping of magnesium and nitrogen has a synergistic effect, so that the adsorption capacity of the activated carbon on carbon dioxide is improved.
3. According to the invention, the hemp core is used as a raw material, the reutilization of the biomass waste is realized, and the prepared activated carbon has a unique microstructure of a macroporous-mesoporous-microporous three-dimensional composite hole, large specific surface area and good repeatability.
Drawings
FIG. 1 is a scanning electron microscope image of a hemp core raw material used in the present invention, and (a) a cross section and (b) a longitudinal section of a hemp core.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited thereto.
Example 1:
a preparation method of magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon comprises the following steps: the method comprises the following specific steps: cleaning hemp core (shown in figure 1 of scanning electron microscope) with distilled water, oven drying at 100 deg.C, and cutting into small segments of about 3 cm; soaking the hemp core small segments in a water mixed solution of zinc chloride and magnesium chloride, wherein the concentration of the mixed solution is 50%, the mass ratio of the zinc chloride to the magnesium chloride in the mixed solution is 4:1, and the mass ratio of the zinc chloride to the soaked hemp core is 4: 1. The mixture was immersed under reduced pressure in a vacuum oven for 24 hours, filtered and then dried at 80 ℃ for 24 hours. And (3) putting the dried hemp core into a tube furnace, heating to 600 ℃ at the speed of 5 ℃/min in the nitrogen atmosphere, preserving the heat at 600 ℃ for 2h, and then cooling to room temperature in the nitrogen atmosphere. The obtained carbide is soaked in a dilute hydrochloric acid solution (the concentration is 1mol/L), and washed by distilled water after being washed for 12 hours under vacuum and reduced pressure until the pH value is neutral. Filtering, soaking the obtained carbide in an ethanol solution of 2, 6-diaminopyridine (the concentration is 0.3g/ml) under reduced pressure for 6 hours, and drying at 80 ℃ for 24 hours to obtain the magnesium-nitrogen co-doped active carbon. The specific surface area of the activated carbon is as high as 3128m2Per g, to carbon dioxideThe adsorption capacity (25 ℃, 1bar) is up to 5.87 mmol/g.
Example 2:
a preparation method of magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon comprises the following steps: the method comprises the following specific steps: the hemp core is dried at 100 ℃ after being cleaned by distilled water and cut into small sections of 3 cm. The hemp core pieces were immersed in a mixed solution of zinc chloride and magnesium chloride. The concentration of the mixed solution is 50%, the mass ratio of zinc chloride to magnesium chloride in the mixed solution is 4:1, and the mass ratio of zinc chloride to the dipped hemp core is 2: 1. The mixture was immersed under reduced pressure in a vacuum oven for 24 hours, filtered and then dried at 80 ℃ for 24 hours. And (3) placing the dried hemp core in a tube furnace, heating to 800 ℃ at the speed of 5 ℃/min in the nitrogen atmosphere, preserving the heat for 2h at 800 ℃, and then cooling to room temperature in the nitrogen atmosphere. The obtained carbide is soaked in a dilute hydrochloric acid solution (the concentration is 1mol/L), and washed by distilled water after being washed for 12 hours under vacuum and reduced pressure until the pH value is neutral. After filtration, the obtained carbide is immersed in an ethanol solution of 2-aminopyridine (the concentration is 0.5g/ml) under reduced pressure for 6 hours, and then dried at 80 ℃ for 24 hours to obtain the magnesium-nitrogen co-doped active carbon. The specific surface area of the activated carbon is up to 2930m2The adsorption capacity to carbon dioxide (25 ℃, 1bar) is up to 5.49 mmol/g.
Claims (6)
1. A preparation method of magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon is characterized by comprising the following steps: the method comprises the following steps:
(1) cleaning and drying hemp core, and cutting into small sections;
(2) placing the hemp core small segments into a mixed aqueous solution of zinc chloride and magnesium chloride, fully soaking, filtering, and drying at 78-82 ℃ for 12-26 h;
(3) sintering the dried hemp core small sections at high temperature under the protection of inert gas, preserving the heat for a period of time, and then naturally cooling under the protection of inert gas to obtain carbide;
(4) washing the carbide with vacuum reduced pressure acid for 10-14h, and washing with distilled water to reach neutral pH;
(5) fully soaking the carbide obtained in the step (4) in an ethanol solution of an aminopyridine compound, and drying at 78-82 ℃ for 12-26h to obtain the magnesium-nitrogen co-doped high-specific-surface-area biomass activated carbon;
in the step (2), the concentration of the mixed solution of zinc chloride and magnesium chloride in the mixed aqueous solution is 20-60%; the mass ratio of zinc chloride to magnesium chloride in the mixed aqueous solution is 1:1-4:1, the mass ratio of zinc chloride to the soaked hemp core is 2:1-4:1, and the soaking time of the hemp core is 18-48 h;
in the step (5), the concentration of the aminopyridine compound in the ethanol solution of the aminopyridine compound is 0.2-0.5 g/ml; the dipping time is 4h-12 h.
2. A process for preparing a magnesium nitrogen co-doped high specific surface area biomass activated carbon as claimed in claim 1, wherein: in the step (1), the drying temperature after cleaning is 98-102 ℃, and the hemp core is cut into small sections with the length of 1-5 cm.
3. A process for preparing a magnesium nitrogen co-doped high specific surface area biomass activated carbon as claimed in claim 1, wherein: in the step (3), the inert gas is nitrogen or argon.
4. A process for preparing a magnesium nitrogen co-doped high specific surface area biomass activated carbon as claimed in claim 1: the method is characterized in that: in the step (3), the high-temperature sintering and heat preservation for a period of time are as follows: heating to 900 ℃ at the speed of 5-10 ℃/min for high-temperature sintering, and keeping the temperature for 2-5 h.
5. A process for preparing a magnesium nitrogen co-doped high specific surface area biomass activated carbon as claimed in claim 1, wherein: in the step (4), the acid used for the acid washing is one or more of diluted hydrochloric acid, diluted sulfuric acid or diluted nitric acid.
6. A process for preparing a magnesium nitrogen co-doped high specific surface area biomass activated carbon as claimed in claim 1, wherein: in the step (5), the aminopyridine compound is more than one of 2-aminopyridine, 2, 3-diaminopyridine and 2, 6-diaminopyridine.
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CN106902742A (en) * | 2017-04-26 | 2017-06-30 | 中南大学 | A kind of porous activated carbon supported magnesium oxide composite and its preparation method and application |
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CN108854432A (en) * | 2018-07-17 | 2018-11-23 | 张玉英 | A kind of active carbon removing formaldehyde/bacteria cellulose compounded mix and preparation method |
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CN101181993A (en) * | 2007-12-13 | 2008-05-21 | 中国人民解放军总后勤部军需装备研究所 | Kenaf stalk activated charcoal and preparation method thereof |
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