CN116375031A - Low-temperature activated carbon, preparation method and application - Google Patents
Low-temperature activated carbon, preparation method and application Download PDFInfo
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- CN116375031A CN116375031A CN202310411232.5A CN202310411232A CN116375031A CN 116375031 A CN116375031 A CN 116375031A CN 202310411232 A CN202310411232 A CN 202310411232A CN 116375031 A CN116375031 A CN 116375031A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 239000012190 activator Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 238000000746 purification Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 238000007639 printing Methods 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 239000011232 storage material Substances 0.000 claims abstract description 5
- 239000007772 electrode material Substances 0.000 claims abstract description 4
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 57
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 14
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 12
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 12
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000012265 solid product Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 10
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- VUFOSBDICLTFMS-UHFFFAOYSA-M ethyl-hexadecyl-dimethylazanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)CC VUFOSBDICLTFMS-UHFFFAOYSA-M 0.000 claims description 8
- 238000010000 carbonizing Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- MLPVBIWIRCKMJV-UHFFFAOYSA-N 2-ethylaniline Chemical compound CCC1=CC=CC=C1N MLPVBIWIRCKMJV-UHFFFAOYSA-N 0.000 claims description 6
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 6
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- ZWAPMFBHEQZLGK-UHFFFAOYSA-N 5-(dimethylamino)-2-methylidenepentanamide Chemical compound CN(C)CCCC(=C)C(N)=O ZWAPMFBHEQZLGK-UHFFFAOYSA-N 0.000 claims description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 4
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- FTZQXOJYPFINKJ-UHFFFAOYSA-N 2-fluoroaniline Chemical compound NC1=CC=CC=C1F FTZQXOJYPFINKJ-UHFFFAOYSA-N 0.000 claims description 3
- QSNSCYSYFYORTR-UHFFFAOYSA-N 4-chloroaniline Chemical compound NC1=CC=C(Cl)C=C1 QSNSCYSYFYORTR-UHFFFAOYSA-N 0.000 claims description 3
- KRZCOLNOCZKSDF-UHFFFAOYSA-N 4-fluoroaniline Chemical compound NC1=CC=C(F)C=C1 KRZCOLNOCZKSDF-UHFFFAOYSA-N 0.000 claims description 3
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 3
- AFBPFSWMIHJQDM-UHFFFAOYSA-N N-methylaniline Chemical compound CNC1=CC=CC=C1 AFBPFSWMIHJQDM-UHFFFAOYSA-N 0.000 claims description 3
- 239000003463 adsorbent Substances 0.000 claims description 3
- -1 carbamyl disodium phosphate Chemical compound 0.000 claims description 3
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 3
- 235000019800 disodium phosphate Nutrition 0.000 claims description 3
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- BTAAXEFROUUDIL-UHFFFAOYSA-M potassium;sulfamate Chemical compound [K+].NS([O-])(=O)=O BTAAXEFROUUDIL-UHFFFAOYSA-M 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- QDWYPRSFEZRKDK-UHFFFAOYSA-M sodium;sulfamate Chemical compound [Na+].NS([O-])(=O)=O QDWYPRSFEZRKDK-UHFFFAOYSA-M 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims description 2
- 238000004146 energy storage Methods 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000000976 ink Substances 0.000 claims 1
- 239000002063 nanoring Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- 239000003054 catalyst Substances 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000000969 carrier Substances 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 238000004042 decolorization Methods 0.000 abstract description 3
- 238000012983 electrochemical energy storage Methods 0.000 abstract description 3
- 239000004519 grease Substances 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000004913 activation Effects 0.000 abstract description 2
- 238000004887 air purification Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical group C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000000877 morphologic effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- KYXOYPPMBYKBFL-UHFFFAOYSA-M sodium;2-aminobenzenesulfonate Chemical compound [Na+].NC1=CC=CC=C1S([O-])(=O)=O KYXOYPPMBYKBFL-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000010902 straw Substances 0.000 description 2
- 125000004306 triazinyl group Chemical group 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical class [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000002194 amorphous carbon material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 229940115457 cetyldimethylethylammonium bromide Drugs 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910000474 mercury oxide Inorganic materials 0.000 description 1
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention provides low-temperature activated carbon, a preparation method and application thereof, belongs to the field of activated carbon nano materials, adopts common and easily available industrial grade products as raw materials, has simple equipment and simple preparation process, has strong repeatability and is beneficial to industrialized mass production. The low-temperature activated carbon provided by the invention has relatively low activation temperature and relatively low corrosion of an activator to equipment, further reduces the cost of products, is friendly to the human body and environment, and can be applied to the fields of water treatment, chemical catalysts and carriers, solvent recovery, grease decolorization, air purification and the like in a large scale. Compared with the existing active carbon sold in the market, the product prepared by the invention has large specific surface area, more developed pore structure and less iron content. In addition, the product of the invention can be used in the fields of heavy metal ion adsorption in aqueous solution, automobile tail gas purification, impurity removal of printing ink, gas separation, super capacitor electrode materials, other electrochemical energy storage materials and the like.
Description
Technical Field
The invention belongs to the field of activated carbon nano materials, and particularly relates to low-temperature activated carbon, a preparation method and application thereof.
Background
The active carbon is a black porous solid material, the main component is carbon, and the active carbon contains a small amount of elements such as oxygen, hydrogen, sulfur, nitrogen, chlorine and the like. Because the activated carbon has rich pore structures and huge specific surface area, has no toxic or side effect and secondary pollution, is a high-efficiency adsorption material which is widely accepted in the world at present, can effectively adsorb harmful gases and peculiar smell, and is considered as a most environment-friendly treatment product in treating indoor pollution. In addition, the activated carbon has the characteristics of catalysis, flexibility, wear resistance, conductivity and the like, and is widely applied to the fields of water treatment, chemical catalysts and carriers, gas purification, solvent recovery, grease decolorization, gold extraction, tail liquid recovery, automobile tail gas purification, impurity removal of printing ink, gas separation, electrochemical energy storage materials and the like.
For example, chinese patent No. CN202110058052.4 discloses a method for preparing microporous polymer-derived nitrogen-enriched porous activated carbon adsorbent, which comprises preparing Kong Huohua by high-temperature carbonization and potassium hydroxide by taking continuous rigid biphenyl structure in molecular chain of triazinyl crosslinked microporous polymer as carbon source and triazinyl ring structure as nitrogen source, and preparing Cu-enriched porous activated carbon adsorbent 2+ The isophtalmic metal ions have excellent pore adsorption characteristics. Chinese patent CN202110846095.9 discloses a method for preparing activated carbon from straw, which uses zinc oxide as an activator, and comprises heating straw particles and zinc oxide under nitrogen atmosphere to react, adding phosphoric acid, carbonizing at high temperature, and post-treating with hydrochloric acid to obtain activated carbon with good adsorption property. The Chinese patent No. 201510868434.8 provides a method for preparing active carbon by activating KOH solid, which comprises grinding KOH solid into powder, adding active carbon precursor, calcining at 700-1000deg.C under nitrogen atmosphere for carbonization, washing with water, and oven drying. Although the activated carbon prepared by the patent has better quality, zinc oxide or KOH is used as an activator to make the reaction temperature higher, the energy consumption in the reaction process is larger, and the KOH has serious corrosion to equipment.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides low-temperature activated carbon, a preparation method and application.
In order to achieve the purpose, the invention is realized by adopting the following technical scheme:
the preparation method of the low-temperature activated carbon comprises the following steps:
1) The polymer precursor and benzoyl peroxide are mixed according to a mole ratio of 1: (0.1-0.6) adding into hydrochloric acid with the mass fraction of 3.5%, then adding hexadecyl dimethyl ethyl ammonium bromide to obtain a reaction solution, reacting the reaction solution at the temperature of 0-3 ℃ for 4-12 hours, and collecting a solid product for washing and drying after the reaction is finished;
2) Pre-carbonizing the dried product in nitrogen atmosphere at 380-480 ℃ for 1-1.5 hours, and grinding the product;
3) Uniformly mixing the product with an activator according to the mass ratio of 1 (0.8-1.8), calcining under the nitrogen atmosphere at the calcining temperature of 380-550 ℃ for 1.5-2 hours, and after the calcining, sequentially carrying out acid washing and water washing on the collected solid product, and drying to obtain the active carbon product.
Further, the polymer precursor in the step (1) is vinyl pyrrolidone, pyrrole, methyl acrylate, ethyl acrylate, 2-methyl methacrylate, 2-ethyl methacrylate, acrylamide, methacrylamide, dimethylaminopropyl acrylamide, aniline, p-chloroaniline, 2-fluoroaniline, 4-fluoroaniline, methylaniline or 2-ethylaniline.
Further, the concentration of benzoyl peroxide in the reaction liquid in the step (1) is 0.1-0.5 mol/L.
Further, the concentration of cetyl dimethyl ethyl ammonium bromide is 0.01 to 0.1mol/L.
Further, in the step (3), the activator is carbamyl disodium phosphate, sodium sulfamate, sodium aminobenzenesulfonate, diformylamido sodium or potassium sulfamate.
The low-temperature activated carbon is prepared by the method.
Further, the material is in a nano circular ring shape.
Further, a large number of micropores and mesopores are distributed in the low-temperature activated carbon.
Further, the catalyst is used as an adsorption material for heavy metal ion adsorption in aqueous solution, automobile tail gas purification, impurity removal and gas separation of printing ink; or/and (or)
As supercapacitor electrode material or energy storage material.
Compared with the prior art, the invention has the following beneficial effects:
the raw materials used in the low-temperature activated carbon, the preparation method and the application are common and easily available industrial-grade products, the equipment is simple, the preparation process is simple and convenient, the repeatability is high, and the industrial mass production is facilitated.
The low-temperature activated carbon provided by the invention has relatively low activation temperature and relatively low corrosion of an activator to equipment, further reduces the cost of products, is friendly to the human body and environment, and can be applied to the fields of water treatment, chemical catalysts and carriers, solvent recovery, grease decolorization, air purification and the like in a large scale. Compared with the prior commercial active carbon, the invention has the following beneficial effects that the specific surface area of the product is large, the pore structure is more developed, and the iron content of the product is less. In addition, the product prepared by the invention has clear morphological characteristics, is in a circular ring shape, the diameter of the circular ring is about 200nm, the diameter of a single product is about 50nm, and the whole product has a relatively obvious pore canal structure and can be also used in the fields of heavy metal ion adsorption in aqueous solution, automobile tail gas purification, impurity removal of printing ink, gas separation, supercapacitor electrode materials, other electrochemical energy storage materials and the like.
Drawings
FIG. 1 is a scanning electron microscope image of an activated carbon of example 1;
FIG. 2 is a transmission electron microscope image of the activated carbon of example 1;
FIG. 3 is an XRD pattern for activated carbon of example 1;
FIG. 4 is a graph of isothermal adsorption and desorption of activated carbon nitrogen in example 1;
FIG. 5 is a graph showing the performance of the inventive product for use in a supercapacitor;
table 1 shows the comparison of the activated carbon product prepared according to the present invention with the commercial products;
table 2 shows the Cu content of the aqueous solution of the product of the invention 2+ Adsorption test of (2).
Detailed Description
In order that those skilled in the art will better understand the present invention, a technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in which it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and the claims of the present invention and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that the embodiments of the invention described herein may be implemented in sequences other than those illustrated or otherwise described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the attached drawing figures:
example 1
Methyl acrylate and benzoyl peroxide are mixed according to a mole ratio of 1:0.6 is added into 100mL hydrochloric acid with the mass fraction of 3.5%, the concentration of benzoyl peroxide in the mixed solution is 0.5mol/L, then hexadecyldimethyl ethyl ammonium bromide with the concentration of 0.1mol/L is added, the mixture is stirred to react for 12 hours at the normal pressure and the temperature of 3 ℃, and after the reaction is finished, the collected solid product is washed with deionized water for 3 times and dried at the temperature of 80 ℃. Pre-carbonizing the dried product in nitrogen atmosphere at 480 ℃ for 1.5 hours, and grinding the product for 1.5 hours; uniformly mixing the product with the carbamyl disodium phosphate according to the mass ratio of 1:1.8, calcining under the nitrogen atmosphere at 550 ℃ for 2 hours, washing the collected solid product with dilute hydrochloric acid and deionized water for 3 times respectively after the calcining is finished, and drying to obtain the active carbon product.
Referring to fig. 1, fig. 1 is a scanning electron microscope image of an activated carbon prepared in example 1, the product has clear morphological characteristics, is in a circular ring shape, the diameter of the circular ring is about 200nm, the diameter of a single product is about 50nm, and the whole product has a relatively obvious pore structure.
Referring to fig. 2, fig. 2 is a transmission electron microscope image of the product of example 1, which can be determined to be a typical amorphous carbon material.
Referring to fig. 3, fig. 3 is an XRD pattern of the product of example 1, from which it can be determined that the main component of the product is a carbon material.
Referring to fig. 4, fig. 4 is a nitrogen isothermal adsorption/desorption curve of the product of example 1, which is a typical type I curve, and at a lower relative pressure, the nitrogen adsorption amount increases sharply, indicating that a large number of micropores exist in the product. The product curve is convex upward, which indicates that a certain amount of mesopores exist in the product.
Referring to fig. 5, fig. 5 is an electrochemical performance test chart of the product of example 1. And taking the prepared product as a working electrode of the supercapacitor, taking a platinum sheet as a counter electrode, mercury/mercury oxide as a reference electrode and 6M KOH solution as electrolyte, and performing constant current charge and discharge test. FIG. 5a shows that the specific discharge capacity of the product at 1.0A/g can reach 470F/g. FIG. 5b shows that the capacity retention rate of the product after 10000 times of constant current charge and discharge cycles at 10A/g can reach 81%.
Referring to Table 1, table 1 shows that the product prepared by the invention has larger specific surface area, more developed pore structure and less iron content than the commercial product.
TABLE 1 comparison of products prepared according to the invention with commercially available products
Referring to Table 2, table 2 shows the effect of the product of the present invention on Cu in an aqueous solution 2+ Adsorption test of (2). Firstly, 100mg/L Cu is prepared by deionized water and copper nitrate 2+ Adding 150mg of the product prepared by the method into a standard solution, uniformly stirring, adsorbing for 4 hours, and detecting Cu by using an ultraviolet-visible spectrophotometer 2+ And calculates the concentration of product to Cu 2+ Is not limited, and the adsorption rate of the catalyst is not limited.
TABLE 2 preparation of product according to the invention for Cu 2+ Adsorption test of (2)
Example 2
The ethyl acrylate and benzoyl peroxide are mixed according to a mole ratio of 1:0.1 is added into 60mL hydrochloric acid with the mass fraction of 3.5%, the concentration of benzoyl peroxide in the mixed solution is 0.1mol/L, then hexadecyldimethyl ethyl ammonium bromide with the concentration of 0.01mol/L is added, the mixture is stirred to react for 4 hours at the normal pressure and the temperature of 0 ℃, and after the reaction is finished, the collected solid product is washed with deionized water for 3 times and dried at the temperature of 80 ℃. Pre-carbonizing the dried product in nitrogen atmosphere at 380 ℃ for 1 hour, and grinding the product for 1 hour; uniformly mixing the product with sodium sulfamate according to the mass ratio of 1:0.8, calcining under nitrogen atmosphere at 380 ℃ for 1.5 hours, washing the collected solid product with dilute hydrochloric acid and deionized water for 3 times respectively after the calcining is finished, and drying to obtain the active carbon product.
Example 3
The method comprises the following steps of (1) mixing methacrylamide with benzoyl peroxide: 0.5 is added into 90mL hydrochloric acid with the mass fraction of 3.5%, the concentration of benzoyl peroxide in the mixed solution is 0.4mol/L, then hexadecyldimethyl ethyl ammonium bromide with the concentration of 0.09mol/L is added, the mixture is stirred to react for 11 hours at the normal pressure of 2 ℃, and after the reaction is finished, the collected solid product is washed with deionized water for 3 times and dried at 80 ℃. Pre-carbonizing the dried product in nitrogen atmosphere at 480 ℃ for 1.5 hours, and grinding the product for 1 hour; uniformly mixing the product with sodium aminobenzenesulfonate according to the mass ratio of 1:1.8, calcining under nitrogen atmosphere at 500 ℃ for 2 hours, washing the collected solid product with dilute hydrochloric acid and deionized water for 3 times respectively after calcining, and drying to obtain the active carbon product.
Example 4
The dimethylaminopropyl acrylamide and benzoyl peroxide are mixed according to the mole ratio of 1:0.4 is added into 80mL hydrochloric acid with the mass fraction of 3.5%, the concentration of benzoyl peroxide in the mixed solution is 0.4mol/L, then hexadecyldimethyl ethyl ammonium bromide with the concentration of 0.08mol/L is added, the mixture is stirred to react for 10 hours at the normal pressure and the temperature of 3 ℃, and after the reaction is finished, the collected solid product is washed with deionized water for 3 times and dried at the temperature of 80 ℃. Pre-carbonizing the dried product in nitrogen atmosphere at 480 ℃ for 1.5 hours, and grinding the product for 1 hour; uniformly mixing the product with potassium sulfamate according to the mass ratio of 1:1.8, calcining under nitrogen atmosphere at 550 ℃ for 2 hours, washing the collected solid product with dilute hydrochloric acid and deionized water for 3 times respectively after the calcining is finished, and drying to obtain the active carbon product.
Methyl acrylate, ethyl acrylate, methacrylamide and dimethylaminopropyl acrylamide in examples 1-4 may be replaced with vinylpyrrolidone, pyrrole, methyl 2-methacrylate, ethyl 2-methacrylate, acrylamide, aniline, p-chloroaniline, 2-fluoroaniline, 4-fluoroaniline, methylaniline and 2-ethylaniline.
The above is only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited by this, and any modification made on the basis of the technical scheme according to the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. The preparation method of the low-temperature activated carbon is characterized by comprising the following steps of:
1) The polymer precursor and benzoyl peroxide are mixed according to a mole ratio of 1: (0.1-0.6) adding into hydrochloric acid with the mass fraction of 3.5%, then adding hexadecyl dimethyl ethyl ammonium bromide to obtain a reaction solution, reacting the reaction solution at the temperature of 0-3 ℃ for 4-12 hours, and collecting a solid product for washing and drying after the reaction is finished;
2) Pre-carbonizing the dried product in nitrogen atmosphere at 380-480 ℃ for 1-1.5 hours, and grinding the product;
3) Uniformly mixing the product with an activator according to the mass ratio of 1 (0.8-1.8), calcining under the nitrogen atmosphere at the calcining temperature of 380-550 ℃ for 1.5-2 hours, and after the calcining, sequentially carrying out acid washing and water washing on the collected solid product, and drying to obtain the active carbon product.
2. The method for preparing activated carbon at low temperature according to claim 1, wherein the polymer precursor in the step (1) is vinyl pyrrolidone, pyrrole, methyl acrylate, ethyl acrylate, 2-methyl methacrylate, 2-ethyl methacrylate, acrylamide, methacrylamide, dimethylaminopropyl acrylamide, aniline, p-chloroaniline, 2-fluoroaniline, 4-fluoroaniline, methylaniline or 2-ethylaniline.
3. The method for producing a low-temperature activated carbon according to claim 1, wherein the concentration of benzoyl peroxide in the reaction liquid in the step (1) is 0.1 to 0.5mol/L.
4. The method for preparing low-temperature activated carbon according to claim 1, wherein the concentration of hexadecyldimethyl ethyl ammonium bromide is 0.01-0.1 mol/L.
5. The method for preparing low-temperature activated carbon according to claim 1, wherein in the step (3), the activator is carbamyl disodium phosphate, sodium sulfamate, sodium dicarboxamide or potassium sulfamate.
6. A low temperature activated carbon prepared according to the method of any one of claims 1 to 5.
7. The activated carbon of claim 6, wherein the activated carbon is in the form of a nanoring.
8. The activated carbon of claim 6, wherein said activated carbon comprises a plurality of micropores and mesopores.
9. The use of a low temperature activated carbon as claimed in claim 6, 7 or 8 as an adsorbent for the adsorption of heavy metal ions in aqueous solutions, purification of automobile exhaust gases, removal of impurities from printing inks and gas separation; or/and (or)
As supercapacitor electrode material or energy storage material.
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|---|---|---|---|---|
| CN118125440A (en) * | 2024-05-06 | 2024-06-04 | 长虹三杰新能源有限公司 | Activation method and application of crop straw and lithium battery manufactured by same |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080138526A1 (en) * | 2006-06-09 | 2008-06-12 | Georgia-Pacific Chemicals Llc | Porous fiberglass materials having reduced formaldehyde emissions |
| CN104495833A (en) * | 2015-01-14 | 2015-04-08 | 北京化工大学 | Three-dimensional structure sulfur-nitrogen codope hierarchical pore graphene and preparation method thereof |
| CN107200324A (en) * | 2017-06-27 | 2017-09-26 | 东莞理工学院 | A kind of activated carbon, its preparation method and application |
| CN108751160A (en) * | 2018-06-15 | 2018-11-06 | 华南理工大学 | A kind of uniform lignin porous carbon in duct and preparation method thereof and the application in lithium ion battery negative material |
| CN115490232A (en) * | 2022-11-02 | 2022-12-20 | 江西省科学院应用化学研究所 | Nitrogen-sulfur co-doped or sulfur-doped porous carbon material and preparation method and application thereof |
-
2023
- 2023-04-17 CN CN202310411232.5A patent/CN116375031A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080138526A1 (en) * | 2006-06-09 | 2008-06-12 | Georgia-Pacific Chemicals Llc | Porous fiberglass materials having reduced formaldehyde emissions |
| CN104495833A (en) * | 2015-01-14 | 2015-04-08 | 北京化工大学 | Three-dimensional structure sulfur-nitrogen codope hierarchical pore graphene and preparation method thereof |
| CN107200324A (en) * | 2017-06-27 | 2017-09-26 | 东莞理工学院 | A kind of activated carbon, its preparation method and application |
| CN108751160A (en) * | 2018-06-15 | 2018-11-06 | 华南理工大学 | A kind of uniform lignin porous carbon in duct and preparation method thereof and the application in lithium ion battery negative material |
| CN115490232A (en) * | 2022-11-02 | 2022-12-20 | 江西省科学院应用化学研究所 | Nitrogen-sulfur co-doped or sulfur-doped porous carbon material and preparation method and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| LIFENG ZHANG ET AL: ""Ion-matching porous carbons with ultra-high surface area and superior energy storage performance for supercapacitors"", 《JOURNAL OF MATERIALS CHEMISTRY A》, vol. 7, no. 15, 21 March 2019 (2019-03-21), pages 9163 - 9172 * |
| YU GUO ET AL: ""Almond Shell-Derived Carbons under Low-Temperature Activation with Ultra-High Surface Area and Superior Performance for Supercapacitors"", 《ENERGY TECHNOLOGY & ENVIRONMENTAL SCIENCE》, vol. 4, no. 43, 26 November 2019 (2019-11-26), pages 12472 - 12478 * |
| 冯小童: ""新型掺杂多孔碳材料的合成、调控及其电化学性能"", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》, 15 February 2020 (2020-02-15), pages 015 - 13 * |
| 展学成;邹欣;马好文;王斌;胡晓丽;孙利民;郑云弟;: "石墨烯基催化剂及其催化加氢应用研究进展", 石化技术与应用, no. 02, 10 March 2017 (2017-03-10) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118125440A (en) * | 2024-05-06 | 2024-06-04 | 长虹三杰新能源有限公司 | Activation method and application of crop straw and lithium battery manufactured by same |
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