CN101244819A - Method for manufacturing metallic absorbent charcoal - Google Patents
Method for manufacturing metallic absorbent charcoal Download PDFInfo
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- CN101244819A CN101244819A CN 200710118215 CN200710118215A CN101244819A CN 101244819 A CN101244819 A CN 101244819A CN 200710118215 CN200710118215 CN 200710118215 CN 200710118215 A CN200710118215 A CN 200710118215A CN 101244819 A CN101244819 A CN 101244819A
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- absorbent charcoal
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- metallic absorbent
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- 239000002250 absorbent Substances 0.000 title claims description 31
- 230000002745 absorbent Effects 0.000 title claims description 31
- 239000003610 charcoal Substances 0.000 title claims description 31
- 238000000034 method Methods 0.000 title description 15
- 238000004519 manufacturing process Methods 0.000 title 1
- 238000002360 preparation method Methods 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 239000012190 activator Substances 0.000 claims abstract description 10
- 239000003245 coal Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 229910000765 intermetallic Inorganic materials 0.000 claims description 17
- 239000011280 coal tar Substances 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000013543 active substance Substances 0.000 claims description 5
- 239000010949 copper Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 230000004913 activation Effects 0.000 claims description 4
- 235000011089 carbon dioxide Nutrition 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 239000000295 fuel oil Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- 235000013379 molasses Nutrition 0.000 claims description 3
- 239000011295 pitch Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 13
- 239000002184 metal Substances 0.000 abstract description 12
- 239000011148 porous material Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 10
- 229910052799 carbon Inorganic materials 0.000 abstract description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract 1
- 239000001569 carbon dioxide Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 239000003990 capacitor Substances 0.000 description 15
- 239000007772 electrode material Substances 0.000 description 10
- 239000012752 auxiliary agent Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 8
- 239000002802 bituminous coal Substances 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- -1 maximum rutheniums Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
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- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method for metal active carbon used in electrodes, which is characterized in that coal is used as raw material, metal compounds, binder and surfactant are added, uniformly mixed, layered and molded to get strip. After being dried, the strip is carbonized under certain temperature and activated with steam, carbon dioxide or the mixtures as activator under a certain temperature to get metal active carbon at last. The preparation method for electrode metal active carbon has the advantages of rich material resources and low price, and thus can be used to prepare metal active carbon with abundant pores, controllable pore structure, large quantity of mesopores, and double effects of double-layer capacitance and quasi-capacitance.
Description
Technical field
The present invention relates to the Preparation of Activated Carbon field, relate in particular to the preparation method of a kind of electrode for capacitors with metallic absorbent charcoal.
Background technology
Ultracapacitor (electrochemical capacitor) is a kind of between store battery and traditional capacitor, based on the energy-storage travelling wave tube of the electrochemical process at electrode/electrolyte interface.Its capacity derives from electric double layer capacitance and pseudo capacitance, it has the big and high characteristics of storage battery energy density of ordinary capacitor power density concurrently, have excellence continuous fast charging and discharging performance, have extended cycle life, use temperature wide ranges, non-maintaining, advantages of environment protection.Ultracapacitor all has wide practical use in a lot of fields, as aerospace, military affairs, industry, civil area or be used to adjust electric load separately, store electric power, or mix use with the device of generation electric energy such as fuel cell, solar cell, wind-power electricity generation, oil engine.
Studies show that the electrode materials of ultracapacitor is one of key factor of its performance of restriction, the electrode materials as ultracapacitor mainly is porous carbon material and metal oxide and hydrate thereof at present.
What porous carbon material mainly produced is electric double layer capacitance, because of its stable performance, existing donor state have acceptor state, environmental friendliness again, more application is in capacitor electrode material, particularly the gac that cost is cheap relatively has flourishing hole, great surface-area, can adsorb more electrolyte ion, storage more energy with its preparation electrode, become the main raw material of preparation of industrialization electrode of super capacitor.Yet electrode active carbon is comparatively harsh to the research of pore structure: micropore (<2nm) be main gac, because its hole is less, be unfavorable for the quick travel of electrolyte ion, make that the surface-area utilization ratio is lower, the low temperature capacity is affected; Mesopore activated carbon (though>2nm) its hole helps the quick travel of electrolytic solution, and the rapid large-current discharge performance is superior, and specific surface area is less relatively, and energy stored is also less, influences its energy density and power density.So have more mesopore concurrently and be the preferred material of making electrode than the gac of bigger serface.
The main effect of metal oxide and hydrate thereof is to produce pseudo capacitance, and some metallic compounds are (as RuO
2XH
2O etc.) and electrolytic solution redox reaction can take place on its surface, electrode is by the reaction of faraday's electrode fast stored energy.At present, the ratio electric capacity of studying compounds such as maximum rutheniums, iridium is higher, but is noble metal, is difficult to bear on price; Compounds such as some cheap metals such as copper, cobalt, nickel, manganese also have the pseudo-capacitance phenomenon to take place, but it is lower than electric capacity, influences practical application.
For improving electrode performance, it is the more method of studying at present that the finished product gac is carried out blended metal oxide, and it can take into account the pseudo-capacitance effect of the electric double layer capacitance and the metal of gac.As: people such as Ling Licheng are in patent " a kind of doping cheap metal improves mesopore activated carbon and compares capacitive method; publication number CN1410350A ", a kind of method for preparation of active carbon of blended metal oxide is provided, it specifically is source from the preparation gac, consider directly to utilize resol, cheap organic metal salt, ferrocene, hexamethylenetetramine, methanol mixed, stirring and refluxing is cured, processing step such as charing and activation makes electrode active carbon again.Though this method has played certain effect, it is higher to have cost of material equally, and the source is restricted, the problem of the loaded down with trivial details harshness of preparation technology.
Summary of the invention
In view of the existing in prior technology problem, embodiment of the present invention provides the preparation method of a kind of electrode with metallic absorbent charcoal.
Embodiment of the present invention is achieved through the following technical solutions:
A kind of preparation method of metallic absorbent charcoal comprises step:
A: with metallic compound, coal raw materials, binding agent and tensio-active agent thorough mixing, press strip and drying;
B: with dried material bar 400~700 ℃ of following charings;
C: be that activator is 700~1000 ℃ of activation down to contain mixture of steam again.
Wherein, the described metallic compound of steps A is the transistion metal compound that comprises at least a manganese, copper, nickel, cobalt, iron etc.; Described metallic compound is Powdered or solution.
The described metallic compound of steps A, coal raw materials, binding agent and the well-mixed ratio of tensio-active agent are: (1~40): 100: (25~65): (0.1~1) (weight); Wherein the ratio of metallic compound is to calculate with the weight of metallic element.
Step B further comprises: with dried material bar 400~700 ℃ of charings 0.5~2.5 hour.
Step C further comprises: be that activator activates 2~40 hours down at 700~1000 ℃ to contain mixture of steam again.
The described activator of step C further is the mixture that comprises water vapour and/or carbonic acid gas.
The described binding agent of steps A is coal tar, pitch, heavy oil, molasses etc.
By the above-mentioned technical scheme that provides as can be seen, the preparation raw material sources of the described method of embodiment of the present invention are abundant, cheap, the prosperity of gac hole, Controlled Pore Structure, the mesopore amount height of preparation, possess electric double layer capacitance and pseudo-capacitance effect double effects simultaneously, and preparation technology is simple, energy consumption is low.
Description of drawings
Fig. 1 is the schema of the described method of embodiment of the present invention.
Embodiment
Embodiment of the present invention provides the preparation method of a kind of electrode with metallic absorbent charcoal, this method is to be raw material with the coal, by adding metallic compound, binding agent and tensio-active agent, through uniform mixing, press strip, make the material bar, charing at a certain temperature after drying is that activator activates at a certain temperature with water vapour, carbonic acid gas or its mixture again, finally makes required metallic absorbent charcoal.The metallic absorbent charcoal that makes by the described method of embodiment of the present invention can make metallic compound disperse very evenly, promoted the catalytic preparation of gac, make it the time as electrode of super capacitor, both can improve the ratio electric capacity of gac by forming the electrostatic double layer stored charge, also can utilizing the pseudo-capacitance effect of metal remained compound to increase charge storage ability.
For describing embodiment of the present invention better, now in conjunction with the accompanying drawings the specific embodiment of the present invention is described:
Fig. 1 is the schema of the described method of embodiment of the present invention, comprises among the figure:
Step 10: preprocessing process, adopt raw material method such as broken, levigate, obtain solution to carry out pre-treatment.
Step 11: with pretreated raw material thorough mixing, press strip.Raw material described here comprises metallic compound, coal raw material, binding agent and auxiliary agent, and metallic compound wherein is the compound that comprises metals such as at least a manganese, copper, nickel, cobalt, iron.
Feed coal can be selected the coal of different metamorphic grade for use, and binding agent wherein can be selected coal tar, pitch, heavy oil, molasses etc. for use, above-described metallic compound, coal raw material, binding agent and the well-mixed ratio of auxiliary agent can for: (1~40): 100: (25~65): (0.1~1) (weight), the ratio of the metallic compound here are to calculate with the weight of the metallic element that wherein comprises.
Step 12: with the material bar drying behind the press strip.
Step 13: with the charing of dried material bar.The temperature of selecting for use during charing can be under 400~700 ℃, preferably can be with dried mixture at N
2Protect about 45 minutes of following 600 ℃ of charings.
Step 14: carbide is activated comprising under the activator of water vapour.The activator here can be the mixture that comprises water vapour and/or carbonic acid gas, and the activation temperature of choosing is at 700~1000 ℃, preferably can activate 10~30 hours down at 850 ℃.
By above step, can obtain metallic absorbent charcoal.
For further describing embodiment of the present invention, now in conjunction with specific embodiments its technical scheme is described further:
Embodiment 1
Get 100g bituminous coal, 70gMn (NO
3)
2Solution (50w%), 45g coal tar, 0.5g auxiliary agent and an amount of water mix, and mediate stirring, press strip (φ 2mm), dry 12h under 80 ℃ of conditions then.The siccative bar is truncated into length about 20mm,, activates 120 minutes with water vapour down at 850 ℃ again, gained metallic absorbent charcoal BET specific surface area 890m 600 ℃ of following charings 45 minutes
2/ g, total pore volume is 1.28cm
3/ g, it was 328F/g than electric capacity when this metallic absorbent charcoal was used as capacitor electrode material.
Embodiment 2
Get 100g bituminous coal, 140gMn (NO
3)
2Solution (50%w), 45g coal tar, 0.5g auxiliary agent and an amount of water mix, mediate stir, press strip (φ 2mm), under 80 ℃ of conditions dry 12 hours then.The siccative bar is truncated into length about 20mm,, activates 120 minutes with water vapour down at 850 ℃ again, gained metallic absorbent charcoal BET specific surface area 1130m 600 ℃ of following charings 45 minutes
2/ g, total pore volume is 1.16cm
3/ g, it was 301F/g than electric capacity when this metallic absorbent charcoal was used as capacitor electrode material.
Embodiment 3
Get 100g bituminous coal, 62.5gCu (NO
3)
23H
2O (wiring solution-forming), 45g coal tar, 0.5g auxiliary agent and an amount of water mix, mediate stir, press strip (φ 2mm), under 80 ℃ of conditions dry 12 hours then.The siccative bar is truncated into length about 20mm,, activates 120 minutes with water vapour down at 850 ℃ again, gained metallic absorbent charcoal BET specific surface area 922m 600 ℃ of following charings 45 minutes
2/ g, total pore volume is 0.95cm
3/ g, it was 236F/g than electric capacity when this metallic absorbent charcoal was used as capacitor electrode material.
Embodiment 4
Get 100g bituminous coal, 125gCu (NO
3)
23H
2O (wiring solution-forming), 45g coal tar, 0.5g auxiliary agent and an amount of water mix, mediate stir, press strip (φ 2mm), under 80 ℃ of conditions dry 12 hours then.The siccative bar is truncated into length about 20mm,, activates 120 minutes with water vapour down at 850 ℃ again, gained metallic absorbent charcoal specific surface area 1071m 600 ℃ of following charings 45 minutes
2/ g, total pore volume is 1.07cm
3/ g, it was 323.8F/g than electric capacity when this metallic absorbent charcoal was used as capacitor electrode material.
Embodiment 5
Get 100g bituminous coal, 42gNi (NO
3)
23H
2O (wiring solution-forming), 45g coal tar, 0.5g auxiliary agent and an amount of water mix, mediate stir, press strip (φ 2mm), under 80 ℃ of conditions dry 12 hours then.The siccative bar is truncated into length about 20mm,, activates 120 minutes with water vapour down at 850 ℃ again, gained metallic absorbent charcoal specific surface area 746m 600 ℃ of following charings 45 minutes
2/ g, total pore volume is 0.93cm
3/ g, it was 190.8F/g than electric capacity when this metallic absorbent charcoal was used as capacitor electrode material.
Embodiment 6
Get 100g bituminous coal, 84gNi (NO
3)
23H
2O (wiring solution-forming), 45g coal tar, 0.5g auxiliary agent and an amount of water mix, mediate stir, press strip (φ 2mm), under 80 ℃ of conditions dry 12 hours then.The siccative bar is truncated into length about 20mm,, activates 120 minutes with water vapour down at 850 ℃ again, gained metallic absorbent charcoal specific surface area 856m 600 ℃ of following charings 45 minutes
2/ g, total pore volume is 1.09cm
3/ g, it was 273F/g than electric capacity when this metallic absorbent charcoal was used as capacitor electrode material.
Embodiment 7
Get 100g bituminous coal, 101g Mn (NO
3)
2, Cu (NO
3)
2, Ni (NO
3)
2Mixing solutions (1: 1: 1) in metal quality, 45g coal tar, 0.5g auxiliary agent and an amount of water mix, mediate stir, press strip (φ 2mm), under 80 ℃ of conditions dry 12 hours then.The siccative bar is truncated into length about 20mm,, activates 120 minutes with water vapour down at 850 ℃ again, gained metallic absorbent charcoal BET specific surface area 1122m 600 ℃ of following charings 45 minutes
2/ g, total pore volume is 1.48cm
3/ g, it was 345F/g than electric capacity when this metallic absorbent charcoal was used as capacitor electrode material.
In sum, the described method of embodiment of the present invention, its preparation raw material sources are abundant, cheap, the gac hole prosperity of preparation, Controlled Pore Structure, mesopore amount height, possess electric double layer capacitance and pseudo-capacitance effect double effects simultaneously, and preparation technology is simple, energy consumption is low.Simultaneously, the metallic absorbent charcoal that makes by the described method of embodiment of the present invention can make metallic compound disperse very evenly, promoted the catalytic preparation of gac, make it the time as electrode of super capacitor, both can effectively improve the ratio electric capacity of gac by forming the electrostatic double layer stored charge, also can utilizing the pseudo-capacitance effect of metal remained compound to increase charge storage ability.
The above; only be one of preferable embodiment of the present invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the embodiment of the invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (7)
1. the preparation method of a metallic absorbent charcoal is characterized in that, comprises step:
A: with metallic compound, coal raw materials, binding agent and tensio-active agent thorough mixing, press strip and drying;
B: with dried material bar 400~700 ℃ of following charings;
C: be that activator is 700~1000 ℃ of activation down to contain mixture of steam again.
2. the preparation method of metallic absorbent charcoal as claimed in claim 1 is characterized in that, the described metallic compound of steps A is the transistion metal compound that comprises at least a manganese, copper, nickel, cobalt, iron etc.; Described metallic compound is Powdered or solution.
3. the preparation method of metallic absorbent charcoal as claimed in claim 1 or 2, it is characterized in that the described metallic compound of steps A, coal raw materials, binding agent and the well-mixed ratio of tensio-active agent are: (1~40): 100: (25~65): (0.1~1) (weight); Wherein the ratio of metallic compound is to calculate with the weight of metallic element.
4. the preparation method of metallic absorbent charcoal as claimed in claim 1 is characterized in that, step B further comprises: with dried material bar 400~700 ℃ of charings 0.5~2.5 hour.
5. the preparation method of metallic absorbent charcoal as claimed in claim 1 is characterized in that, step C further comprises: be that activator activates 2~40 hours down at 700~1000 ℃ to contain mixture of steam again.
6. the preparation method of metallic absorbent charcoal as claimed in claim 5 is characterized in that, the described activator of step C further is the mixture that comprises water vapour and/or carbonic acid gas.
7. the preparation method of metallic absorbent charcoal as claimed in claim 1 is characterized in that, the described binding agent of steps A be following one or more: coal tar, pitch, heavy oil, molasses.
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CN 200710118215 CN101244819A (en) | 2007-07-02 | 2007-07-02 | Method for manufacturing metallic absorbent charcoal |
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CN105271225A (en) * | 2015-11-05 | 2016-01-27 | 新奥科技发展有限公司 | Preparing method for activated carbon |
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CN111377443B (en) * | 2018-12-29 | 2022-06-07 | 中国石油化工股份有限公司 | Copper-doped activated carbon composite material and preparation method thereof |
CN110018214A (en) * | 2019-05-20 | 2019-07-16 | 中南大学 | A kind of method of modified coal Quito pore electrod measurement ascorbic acid content |
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CN110482544A (en) * | 2019-09-03 | 2019-11-22 | 炬福(福建)环保科技有限公司 | Active carbon and its preparation method and application |
CN110482544B (en) * | 2019-09-03 | 2021-05-28 | 炬福(福建)环保科技有限公司 | Activated carbon and preparation method and application thereof |
CN111204732A (en) * | 2020-01-13 | 2020-05-29 | 吉林大学 | Transition metal doped porous carbon material and preparation method and application thereof |
CN112588263A (en) * | 2020-11-30 | 2021-04-02 | 德清县联新环保科技有限公司 | Regenerated active carbon and preparation method thereof |
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