CN115394566A - Method for purifying active carbon-based material of super-capacitor electrode - Google Patents
Method for purifying active carbon-based material of super-capacitor electrode Download PDFInfo
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- CN115394566A CN115394566A CN202211009889.0A CN202211009889A CN115394566A CN 115394566 A CN115394566 A CN 115394566A CN 202211009889 A CN202211009889 A CN 202211009889A CN 115394566 A CN115394566 A CN 115394566A
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 40
- 239000003990 capacitor Substances 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000012535 impurity Substances 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 8
- 229910052755 nonmetal Inorganic materials 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012466 permeate Substances 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- -1 propylene alcohol Chemical compound 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000005470 impregnation Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
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- 239000000758 substrate Substances 0.000 abstract description 3
- 210000005239 tubule Anatomy 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 28
- 239000000243 solution Substances 0.000 description 12
- 229910021393 carbon nanotube Inorganic materials 0.000 description 8
- 239000002041 carbon nanotube Substances 0.000 description 8
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 235000013162 Cocos nucifera Nutrition 0.000 description 6
- 244000060011 Cocos nucifera Species 0.000 description 6
- 238000004146 energy storage Methods 0.000 description 5
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- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
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- 239000002904 solvent Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010574 gas phase reaction Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910013872 LiPF Inorganic materials 0.000 description 1
- 101150058243 Lipf gene Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 239000000010 aprotic solvent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
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- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention relates to a method for purifying an active carbon-based material of a super-capacitor electrode, which is to clean and remove metal and nonmetal impurities in the active carbon-based material of the super-capacitor electrode by adopting an alcoholic solution of hydrochloric acid. The invention has the beneficial effects that: according to the invention, the hydrochloric acid alcohol solution is adopted to replace the traditional dilute acid water solution for impregnation, the hydrochloric acid alcohol solution has low surface tension, can effectively permeate and diffuse to micropores, mesopores, tubules, complex irregular surfaces, high aspect ratio structures and difficult-to-wet substrates in the carbon-based material, is beneficial to full contact of acid and impurities for reaction, and is relatively thorough in impurity removal.
Description
Technical Field
The invention relates to the field of electrode materials of a super capacitor, in particular to a method for purifying an active carbon-based material of a super capacitor electrode.
Background
Super-capacitor type energy storage devices based on ion adsorption/desorption, such as electric double layer capacitors, battery capacitors and the like, usually use porous carbon-based materials as main or partial electrode active components and tetraethylammonium tetrafluoroborate (TEA-BF) 4 ) Triethylmethylammonium tetrafluoroborate (TEMA-BF) 4 ) Bispyrrolidine spiro quaternary ammonium salt (SBP-BF) 4 ) Lithium hexafluorophosphate (LiPF) 6 ) The electrolyte is dissolved in an aprotic solvent such as acetonitrile or carbonate as an electrolytic solution. Porous carbon-based materials, including activated carbon, microporous carbon, mesoporous carbon, carbon nanotubes, graphene and composite and mixed materials thereof, are one of the most critical factors for determining super capacitive energy storage performance, and have ultralow metal impurity content and high specific surface (difficult to wet) (C)>1500m 2 A/g) and a porous (0.1-50 nm) structure. The metal and non-metal impurities of the porous carbon-based material have obvious influence on super capacitive energy storage using the non-protonized solvent electrolyte, so that not only is the leakage current and the equivalent resistance increased, but also side reactions such as electrolyte decomposition are catalyzed and initiated, and the generated gas can cause the risk of expansion or deformation, burst and the like of a device. This also shortens the life of the super capacitor type energy storage device, especially the charge and discharge cycle stability and life at high voltage or high temperature.
The metal and non-metal impurities in the active carbon-based material of the super capacitor electrode mainly originate from two aspects: inherent raw materials, such as natural products like coconut shells serving as an activated carbon source, and metal and nonmetal impurities contained in coal, petroleum coke and the like; introduction during preparation, e.g. KOH, znCl 2 Activated carbon activators, carbon nanotube growth catalysts such as Fe, co and Ni, mgO and Al 2 O 3 、SiO 2 And the like. The common method for removing metal and non-metal impurities in the active carbon-based material of the super-capacitor electrode is dilute acid impregnation and gas phase reaction. Impregnation with dilute acids (e.g., dilute hydrochloric acid, dilute nitric acid, dilute hydrofluoric acid, dilute sulfuric acid, etc.) is usually combined with aeration, pressurization, and addition of chelateThe means such as the mixture promotes the permeation and diffusion of the cleaning liquid into the porous structure and the reaction and dissolution of impurities, thereby improving the cleaning effect. Because the aqueous solution is difficult to effectively permeate, diffuse and wet micropores, tubules, complex irregular surfaces, high aspect ratio structures and hydrophobic substrates, the cleaning process is long and repeated, impurities in pore cavities are difficult to effectively remove, and the deep purification effect is not ideal. Gas phase reactions typically employ gases (e.g., containing Cl) 2 Gas) and can be quickly diffused and fully contacted with the surfaces difficult to be wetted and the pore channel structure, and partial impurities can be removed after being converted into volatile compounds, but not all the impurities can be converted into the volatile compounds, and the types of the impurities capable of being removed are limited.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for purifying an active carbon-based material of a super-capacitor electrode. The super capacitor electrode made of the super capacitor electrode active carbon-based material is suitable for an electric double layer capacitor, a battery capacitor and other energy storage devices with super capacitor characteristics, wherein the electric double layer capacitor and the battery capacitor use non-protonized solvents such as acetonitrile and carbonic ester as electrolyte solvents.
Preferably, the method for purifying the supercapacitor electrode active carbon-based material comprises the following steps:
s1, soaking a carbon-based material (a porous carbon material) in an alcoholic solution of hydrochloric acid at normal temperature, wherein the alcoholic solution of hydrochloric acid effectively permeates and diffuses to the surface, the pore ports and the interior of the carbon-based material which are difficult to wet and reacts with impurities to generate an alcohol-soluble byproduct;
s2, filtering and separating the carbon-based material, washing the carbon-based material with deionized water for a plurality of times, and drying to obtain the high-purity carbon-based material with ultralow impurity content.
Preferably, in S1, the hydrochloric acid alcohol solution is an organic solvent in which HCl gas is dissolved.
Preferably, in S1, the organic solvent is one or more of methanol, ethanol, n-propanol, isopropanol, propylene alcohol, ethylene glycol, propylene glycol, and glycerol.
Preferably, in S1, the organic solvent contains 0 to 5% of water.
Preferably, in S1, the concentration of HCl in the hydrochloric acid alcohol solution is 0.001 to 2mol/L.
Preferably, in S1, the alcoholic hydrochloric acid solution contains 0 to 500ppm of HF.
Preferably, in S2, the impurity content in the high-purity carbon-based material is: total ash <0.5%, fe <20ppm, K <10ppm, mn <20ppm, cu <20ppm, na <20ppm, ni <20ppm, cr <20ppm, si <20ppm, ca <10ppm, zn <20ppm, zr <20ppm, al <400ppm.
The beneficial effects of the invention are:
(1) According to the invention, the hydrochloric acid alcohol solution is adopted to replace the traditional dilute acid water solution for impregnation, the hydrochloric acid alcohol solution has low surface tension, can effectively permeate and diffuse to micropores, mesopores, tubules, complex irregular surfaces, high aspect ratio structures and difficult-to-wet substrates in the carbon-based material, is beneficial to full contact of acid and impurities for reaction, and is relatively thorough in impurity removal.
(2) The method for purifying the active carbon-based material of the super-capacitor electrode provided by the invention has the advantages of simple process, short cleaning time and high impurity removal rate.
Drawings
FIG. 1 is a comparison graph of the impurity content of coconut shell activated carbon before and after cleaning with an alcoholic solution of hydrochloric acid;
FIG. 2 is a comparison graph of the impurity content of carbon nanotubes before and after washing with an alcoholic solution of hydrochloric acid.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for a person skilled in the art, several modifications can be made to the invention without departing from the principle of the invention, and these modifications and modifications also fall within the protection scope of the claims of the present invention.
Example 1:
soaking coconut shell activated carbon in hydrochloric acid alcohol solution (HCl concentration is 0.001mol/L, HF content is 100 ppm) for 1hr, filtering to separate coconut shell activated carbon, washing with deionized water for several times, and drying to obtain high-purity coconut shell activated carbon with ultralow impurity content. The change of the impurity content of the coconut shell activated carbon before and after cleaning is shown in figure 1. After cleaning, the main metal impurities and the non-metal Si impurities in the activated carbon material can be effectively removed.
Example 2:
soaking carbon nanotube in hydrochloric acid alcohol solution (HCl concentration of 0.002mol/L and HF content of 100 ppm) for 1hr, filtering to separate carbon nanotube, washing with deionized water for several times, and drying to obtain high purity carbon nanotube with ultralow impurity content. The change in the impurity content of the carbon nanotubes before and after the cleaning is shown in FIG. 2. After cleaning, the main metal impurities in the carbon nanotube material can be effectively removed.
In summary, the invention provides a non-aqueous solution cleaning method, which effectively removes metal and non-metal impurities in the active carbon-based material of the supercapacitor electrode, thereby achieving deep purification.
Claims (8)
1. A method for purifying an active carbon-based material of a super-capacitor electrode is characterized in that a hydrochloric acid alcohol solution is adopted for cleaning to remove metal and nonmetal impurities in the active carbon-based material of the super-capacitor electrode.
2. The method for purifying the supercapacitor electrode active carbon-based material according to claim 1, wherein the method for purifying the supercapacitor electrode active carbon-based material comprises the following steps:
s1, soaking a carbon-based material in an alcoholic hydrochloric acid solution at normal temperature, wherein the alcoholic hydrochloric acid solution effectively permeates and diffuses to the surface, pore ports and the interior of the carbon-based material and reacts with impurities to generate an alcohol-soluble byproduct;
and S2, filtering and separating the carbon-based material, washing the carbon-based material with deionized water for a plurality of times, and drying to obtain the high-purity carbon-based material.
3. The method for purifying the supercapacitor electrode active carbon-based material according to claim 2, wherein in S1, the hydrochloric acid alcohol solution is an organic solvent in which HCl gas is dissolved.
4. The method for purifying the supercapacitor electrode active carbon-based material according to claim 3, wherein in S1, the organic solvent is one or more of methanol, ethanol, n-propanol, isopropanol, propylene alcohol, ethylene glycol, propylene glycol and glycerol.
5. The method for purifying the supercapacitor electrode active carbon-based material according to claim 4, wherein in S1, the organic solvent contains 0 to 5 percent of water.
6. The method for purifying the supercapacitor electrode active carbon-based material according to claim 5, wherein in S1, the concentration of HCl in the hydrochloric acid alcohol solution is 0.001-2 mol/L.
7. The method for purifying the supercapacitor electrode active carbon-based material according to claim 6, wherein in S1, the hydrochloric acid alcohol solution contains 0 to 500ppm of HF.
8. The method for purifying the supercapacitor electrode active carbon-based material according to claim 7, wherein in S2, the impurity content in the high-purity carbon-based material is as follows: total ash <0.5%, fe <20ppm, K <10ppm, mn <20ppm, cu <20ppm, na <20ppm, ni <20ppm, cr <20ppm, si <20ppm, ca <10ppm, zn <20ppm, zr <20ppm, al <400ppm.
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| CN202211009889.0A CN115394566B (en) | 2022-08-23 | 2022-08-23 | Purification method of super capacitor electrode active carbon-based material |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101719424A (en) * | 2010-01-12 | 2010-06-02 | 山东理工大学 | Method for preparing micropore carbon material of super capacitor |
| CN102683036A (en) * | 2012-05-02 | 2012-09-19 | 清华大学 | Method for purifying carbon nanometer electrode material of super capacitor |
| CN108069426A (en) * | 2017-09-08 | 2018-05-25 | 山东大学 | A kind of preparation method of ultracapacitor seaweed matrix activated carbon |
| CN111584246A (en) * | 2020-05-19 | 2020-08-25 | 复旦大学 | High-performance supercapacitor negative electrode carbon material and preparation method thereof |
| CN113436900A (en) * | 2021-06-28 | 2021-09-24 | 中南林业科技大学 | Nitrogen-doped carbon-based electrode based on nickel-cobalt double hydroxide, preparation method and super capacitor |
-
2022
- 2022-08-23 CN CN202211009889.0A patent/CN115394566B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101719424A (en) * | 2010-01-12 | 2010-06-02 | 山东理工大学 | Method for preparing micropore carbon material of super capacitor |
| CN102683036A (en) * | 2012-05-02 | 2012-09-19 | 清华大学 | Method for purifying carbon nanometer electrode material of super capacitor |
| CN108069426A (en) * | 2017-09-08 | 2018-05-25 | 山东大学 | A kind of preparation method of ultracapacitor seaweed matrix activated carbon |
| CN111584246A (en) * | 2020-05-19 | 2020-08-25 | 复旦大学 | High-performance supercapacitor negative electrode carbon material and preparation method thereof |
| CN113436900A (en) * | 2021-06-28 | 2021-09-24 | 中南林业科技大学 | Nitrogen-doped carbon-based electrode based on nickel-cobalt double hydroxide, preparation method and super capacitor |
Non-Patent Citations (1)
| Title |
|---|
| 邱家乐: "阵列碳纳米管的两亲性修饰及其应用研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》, no. 2019, 15 April 2019 (2019-04-15), pages 015 - 90 * |
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