CN112456492B - Cleaning method of activated carbon - Google Patents
Cleaning method of activated carbon Download PDFInfo
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- CN112456492B CN112456492B CN202011350520.7A CN202011350520A CN112456492B CN 112456492 B CN112456492 B CN 112456492B CN 202011350520 A CN202011350520 A CN 202011350520A CN 112456492 B CN112456492 B CN 112456492B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 382
- 238000000034 method Methods 0.000 title claims abstract description 84
- 238000004140 cleaning Methods 0.000 title claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 164
- 238000005406 washing Methods 0.000 claims abstract description 102
- 239000002253 acid Substances 0.000 claims abstract description 68
- 238000010438 heat treatment Methods 0.000 claims abstract description 54
- 238000002156 mixing Methods 0.000 claims abstract description 51
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 30
- 230000008569 process Effects 0.000 claims abstract description 30
- 239000003513 alkali Substances 0.000 claims abstract description 28
- 230000002378 acidificating effect Effects 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 47
- 239000008367 deionised water Substances 0.000 claims description 32
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 30
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 13
- 229910017604 nitric acid Inorganic materials 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 150000007513 acids Chemical class 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 26
- 239000012535 impurity Substances 0.000 abstract description 21
- 229910052742 iron Inorganic materials 0.000 abstract description 19
- -1 iron ions Chemical class 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 11
- 229910001453 nickel ion Inorganic materials 0.000 abstract description 11
- 229910001414 potassium ion Inorganic materials 0.000 abstract description 11
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 description 40
- 238000002386 leaching Methods 0.000 description 31
- 230000018044 dehydration Effects 0.000 description 30
- 238000006297 dehydration reaction Methods 0.000 description 30
- 239000000706 filtrate Substances 0.000 description 30
- 238000003825 pressing Methods 0.000 description 25
- 238000005086 pumping Methods 0.000 description 25
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 21
- 239000012065 filter cake Substances 0.000 description 20
- 239000000203 mixture Substances 0.000 description 20
- 239000003990 capacitor Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 238000010907 mechanical stirring Methods 0.000 description 10
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 7
- 238000001994 activation Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 229910052700 potassium Inorganic materials 0.000 description 7
- 239000011591 potassium Substances 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 229910052759 nickel Inorganic materials 0.000 description 6
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- 230000004913 activation Effects 0.000 description 4
- 150000001768 cations Chemical class 0.000 description 4
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 235000014413 iron hydroxide Nutrition 0.000 description 3
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229960004887 ferric hydroxide Drugs 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000276 potassium ferrocyanide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XOGGUFAVLNCTRS-UHFFFAOYSA-N tetrapotassium;iron(2+);hexacyanide Chemical compound [K+].[K+].[K+].[K+].[Fe+2].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] XOGGUFAVLNCTRS-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007833 carbon precursor Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 239000002994 raw material 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
- C01B32/354—After-treatment
- C01B32/378—Purification
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Carbon And Carbon Compounds (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a method for cleaning activated carbon, which belongs to the technical field of activated carbon preparation and comprises the following steps: mixing activated carbon to be cleaned with a first acid solution for neutralization reaction, and dehydrating to obtain neutralized activated carbon; mixing the neutralized activated carbon with the second acid solution, heating to 45-80 ℃ to adjust the pH value to 2-4 to obtain acidic activated carbon; mixing and heating acidic activated carbon and alkali liquor to adjust the pH value to 8-11, and dehydrating to obtain alkali washing activated carbon; and (4) carrying out acid washing and water washing on the alkali washing activated carbon to finish activated carbon cleaning. The content of iron ions in the activated carbon cleaned by the method is 26-88ppm, the content of nickel ions is 2-10ppm, the content of potassium ions is 48-96ppm, the content of impurities is low, and compared with the traditional cleaning mode, the method saves water by more than 35% under similar cleaning effect; the method has the advantages of simple and feasible process, high washing efficiency, low energy consumption, low requirement on equipment, capability of greatly reducing the washing cost and good practicability.
Description
Technical Field
The invention belongs to the technical field of activated carbon preparation, and particularly relates to a method for cleaning activated carbon.
Background
Due to the ultrahigh specific surface area and the developed pore structure, the activated carbon is widely used as an electrode material of a super capacitor and plays an important role in the performance of the super capacitor. Generally, activated carbon is prepared by two methods, physical activation and chemical activation. In order to effectively regulate and control the pore structure of the activated carbon and prepare the activated carbon material with high specific surface area, the activated carbon material is mostly prepared by adopting a KOH high-temperature chemical activation mode at present. Because KOH has extremely strong corrosivity at high temperature, the carbon precursor can be subjected to hole expanding and hole forming efficiently, the process is simple, and the industrial production is easy to realize; however, in the activation process, metal impurities such as iron, nickel, potassium and the like are introduced into the activated carbon due to corrosion of the reaction vessel and equipment, and meanwhile, due to the residue of a large amount of activating agents, the difficulty in cleaning the activated carbon in the later period is increased. The residue of these impurity elements can react in the charging and discharging process of the super capacitor, some of them are even reduced and separated out, which causes short circuit and affects the service life of the super capacitor, and may cause safety problem in severe cases.
In the production and preparation process of the activated carbon for the super capacitor, in order to remove residual impurity elements, the traditional process adopts a mode of acid washing and elutriation. However, because of the strong adsorption capacity of activated carbon to metal impurities, it is difficult to remove the impurities by simple acid immersion cleaning.
Patent CN104118875A discloses a method for cleaning activated carbon by heating a boiling acid solution with steam, which reduces the metal impurities of the activated carbon by repeated cleaning with acid and deionized water by means of strong penetration of steam. Patent CN102874804A adopts multistage acid washing and elutriation, and utilizes a pressurized membrane filtration mode to clean the activated carbon.
Although the above activated carbon cleaning method can remove impurities well, the cleaning process is relatively complex, the energy consumption is high, the requirement on equipment is high, the production efficiency is restricted, and the production cost is increased, so that a new activated carbon cleaning process is urgently needed.
Disclosure of Invention
In order to solve the problems that the cleaning process of the activated carbon is complex, the energy consumption is high, and the requirement on equipment is high in the prior art, so that the production efficiency is restricted, and the production cost is increased, the invention provides the cleaning method of the activated carbon, which has a good impurity removal effect, is simple in process, and is easy to realize industrial production.
The invention provides a method for cleaning activated carbon, which comprises the following steps:
mixing activated carbon to be cleaned with a first acid solution for neutralization reaction, and dehydrating to obtain neutralized activated carbon;
mixing the neutralized activated carbon with a second acid solution, heating to 45-80 ℃, and adjusting the pH value to 2-4 to obtain acidic activated carbon;
mixing the acidic activated carbon with alkali liquor, heating to adjust the pH value to 8-11, and dehydrating to obtain alkali washing activated carbon;
and carrying out acid washing and water washing on the alkali washing activated carbon to finish activated carbon cleaning.
Further, the mixing and heating of the neutralized activated carbon with a second acid solution to 45-80 ℃ comprises,
mixing the neutralized activated carbon with an alcohol solution and a second acid solution, and heating to 45-80 ℃, wherein the mass ratio of the neutralized activated carbon to the alcohol solution is 0.8-1.2: 5-100.
Further, the alcohol solution is any one of the following: the methanol solution and the ethanol solution, wherein the mass fraction of the ethanol solution is less than or equal to 60 percent.
Further, in the neutralization reaction process, the temperature is 45-80 ℃, the stirring speed is 100-500rpm, and the stirring time is 2-12 h; the pH value at the end of the neutralization reaction is 8-10.
Further, in the process of mixing the acidic activated carbon and the alkali liquor, adjusting and adjusting the pH value, heating and stirring are carried out, wherein the heating temperature is 45-80 ℃, the stirring speed is 100-500rpm, and the stirring time is 2-12 h.
Further, the first acid solution is at least one of the following: hydrochloric acid, sulfuric acid and nitric acid, wherein the second acid solution is at least one of the following acids: hydrochloric acid, sulfuric acid, nitric acid.
Further, the alkali liquor is at least one of the following components: potassium hydroxide, sodium hydroxide and ammonia water.
Further, the acid washing is to mix the alkali washing activated carbon with water and add acid liquor to adjust the pH value to 1-2 for acid washing.
Further, the water washing is to mix deionized water and activated carbon, heat and stir, then dehydrate, and repeatedly use deionized water for leaching and dehydration; the heating temperature is 45-80 ℃, the stirring speed is 100-500rpm, and the stirring time is 2-12 h.
Further, the deionized water is water with the resistivity of 0.5-10M omega cm.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
the invention provides a method for cleaning activated carbon, which is characterized in that the activated carbon to be cleaned contains potassium brought by an activating agent, and iron, nickel and the like are introduced by corrosion of a container and equipment in the production and activation processes; firstly, mixing activated carbon to be cleaned with a first acid solution to perform a neutralization reaction, removing a large amount of potassium elements in the form of alkali and salt, then mixing the neutralized activated carbon with a second acid solution, adjusting the pH value to be acidic, and combining iron ions with ferricyanide ions to generate ferric ferrocyanide precipitates, so that the strong adsorption action of the activated carbon and the ferricyanide ions can be destroyed to separate the ferric ferrocyanide ions, then adding alkali solution to adjust the pH value to be alkaline, so that the ferric ferrocyanide can be converted into water-soluble ferrocyanide salts (if the alkali solution is potassium hydroxide, potassium ferrocyanide is generated) and precipitated iron hydroxide, the water-soluble ferrocyanide salts are removed by dehydration, and the remaining impurities such as ferric hydroxide precipitates, nickel, potassium and the like are removed by acid washing and water washing. Test shows that the ash content of the activated carbon cleaned by the method can be reduced to 0.03-0.05%, the iron ion content is 26-88ppm, the nickel ion content is 2-10ppm, the potassium ion content is 48-96ppm, the impurity content is low, and the water is saved by more than 35% compared with the traditional cleaning mode under similar cleaning effect; the method has the advantages of simple and feasible process, high washing efficiency, low energy consumption, low requirement on equipment, capability of greatly reducing the washing cost and good practicability.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
Fig. 1 is a process diagram of an activated carbon cleaning method in embodiment 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In order to solve the technical problems, the embodiment of the invention provides the following general ideas:
the invention provides a method for cleaning activated carbon, which comprises the following steps:
s1, mixing the activated carbon to be cleaned with a first acid solution for neutralization reaction, and dehydrating to obtain neutralized activated carbon;
s2, mixing the neutralized activated carbon with a second acid solution, heating to 45-80 ℃, and adjusting the pH value to 2-4 to obtain acidic activated carbon;
s3, mixing the acidic activated carbon with alkali liquor to adjust the pH value to 8-11, and dehydrating to obtain alkaline washing activated carbon;
s4, performing acid washing and water washing on the alkaline activated carbon to finish activated carbon cleaning.
The invention provides a method for cleaning activated carbon, which is characterized in that the activated carbon to be cleaned contains potassium brought by an activating agent, and iron, nickel and the like are introduced by corrosion of a container and equipment in the production and activation processes; firstly, mixing activated carbon to be cleaned with a first acid solution to perform a neutralization reaction, removing a large amount of potassium elements in the form of alkali and salt, then mixing the neutralized activated carbon with a second acid solution, adjusting the pH value to be acidic, and combining iron ions with ferricyanide ions to generate ferric ferrocyanide precipitates, so that the strong adsorption action of the activated carbon and the ferricyanide ions can be destroyed to separate the ferric ferrocyanide ions, then adding alkali solution to adjust the pH value to be alkaline, so that the ferric ferrocyanide can be converted into water-soluble ferrocyanide salts (if the alkali solution is potassium hydroxide, potassium ferrocyanide is generated) and precipitated iron hydroxide, the water-soluble ferrocyanide salts are removed by dehydration, and the remaining impurities such as ferric hydroxide precipitates, nickel, potassium and the like are removed by acid washing and water washing.
In the step S2, heating is beneficial to the diffusion of molecules, the solubility is increased, and the production efficiency is improved; the pH value is too large, the ferrous cyanide ions can not be precipitated and separated out in the form of ferrous cyanide, the removal effect is poor, the pH value is too small, the removal of iron is not influenced, and excessive acid radical ions can be introduced.
In step S3, the pH value is too large, which does not affect the removal of Fe ions, but can cause the alkali liquor to carry excessive cations; if the pH is too low, the amount of water-soluble ferrocyanide salt formed may be small, and the iron removal effect may be reduced.
As an implementation of the embodiment of the present invention, the mixing and heating the neutralized activated carbon and the second acid solution to 45-80 ℃ comprises,
mixing the neutralized activated carbon with an alcohol solution and a second acid solution, and heating to 45-80 ℃, wherein the mass ratio of the neutralized activated carbon to the alcohol solution is 0.8-1.2: 5-100.
The activated carbon has stronger adsorption capacity to alcohol liquid, can occupy the adsorption site of the activated carbon to the ferrous cyanide ions, and improves the removal effect. The mass ratio of the neutralized activated carbon to the alcohol solution is too large, resulting in poor iron removal effect; if the mass ratio is too small, alcohol solution may be wasted, and the cost may be increased.
As an implementation of the embodiment of the present invention, the alcohol solution includes, but is not limited to, any one of the following: methanol solution and ethanol solution, wherein the mass fraction of the ethanol solution is more than 0 and less than 60 percent.
As an implementation manner of the embodiment of the invention, in the neutralization reaction process, the temperature is 45-80 ℃, the stirring speed is 100-500rpm, and the stirring time is 2-12 h; the pH value at the end of the neutralization reaction is 8-10.
The speed of the neutralization reaction can be improved by controlling the temperature and stirring; the pH at the end of the run was controlled to ensure removal of large amounts of potassium hydroxide.
As an implementation manner of the embodiment of the invention, in the process of adjusting the pH value by mixing the acidic activated carbon and the alkali liquor, heating and stirring are carried out, wherein the heating temperature is 45-80 ℃, the stirring speed is 100-500rpm, and the stirring time is 2-12 h.
The reaction rate can be improved by controlling the heating temperature, the temperature is too high, the water is volatilized too fast, the impurity concentration in the mixed liquid of the activated carbon is high, and the impurities are not easy to dissolve out of the activated carbon.
As an implementation manner of the embodiment of the present invention, the first acid solution includes, but is not limited to, at least one of the following: hydrochloric acid, sulfuric acid, nitric acid, the second acid solution includes but is not limited to at least one of the following: hydrochloric acid, sulfuric acid, nitric acid.
As an embodiment of the present invention, the lye includes but is not limited to at least one of the following: potassium hydroxide, sodium hydroxide and ammonia water.
Although the addition of lye will introduce cations, since lye is not used for activation, the adsorption with activated carbon is not strong and cations are relatively small, so that it can be removed in the subsequent pickling and washing processes.
As an implementation mode of the embodiment of the invention, the acid washing is to mix the alkaline washing activated carbon with water and add acid liquor to adjust the pH value to 1-2 for acid washing.
Nickel and remaining cations can be removed by acid washing, and iron hydroxide that is not removed by the alkaline washing step can also be removed.
As an implementation manner of the embodiment of the invention, the water washing is to mix deionized water and activated carbon, heat and stir, then dehydrate, and repeatedly use deionized water for leaching and dehydration; the heating temperature is 45-80 ℃, the stirring speed is 100-500rpm, and the stirring time is 2-12 h.
As an implementation of the embodiments of the present invention, the deionized water is water having a resistivity of 0.5 to 10M Ω · cm.
In order to further remove impurities, the washing process may be repeated, and the specific washing times may be adjusted according to actual conditions and effects, which is not limited herein. The leaching and the dehydration can also be carried out repeatedly, the leaching frequency can be 5-20 times, and the mass of deionized water used for leaching each time is 3-20 times of that of the activated carbon. In addition, the activated carbon is dehydrated to obtain recovered water after the first water washing, and the recovered water can be used as process water for neutralization reaction because the content of impurities is high. The reclaimed water obtained after the activated carbon is dehydrated after the second water washing, even the third water washing and the fourth water washing can be used as the water for the acid washing process because the impurities are less. The specific application of the recovered water can be adjusted according to the actual situation, and is not limited specifically herein.
The method for cleaning activated carbon according to the present invention will be described in detail with reference to examples, comparative examples and experimental data.
Example 1
Example 1 provides a method for cleaning activated carbon, which is described in detail below with reference to fig. 1:
(1) a neutralization process, namely mixing 3kg of activated carbon with I-grade circulating water according to a mass ratio of 1:20, adding hydrochloric acid to adjust the pH value to 8, heating in a water bath to 60 ℃, adding mechanical stirring at a rotating speed of 200rpm, and stirring for 8 hours to obtain slurry; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating by using I-grade circulating water according to the ratio of 1:10 of the activated carbon to the leacheate for 10 times, feeding the obtained filter cake into an alcohol phase alkaline washing process, and feeding the filtrate into a water treatment system.
(2) Alcohol phase alkali washing process: mixing the activated carbon obtained in the neutralization step with an ethanol solution with the mass fraction of 30% according to the mass ratio of 1:10, adding hydrochloric acid to adjust the pH value to 3, heating in a water bath to 60 ℃, and mechanically stirring at the rotating speed of 200rpm for 2 hours; adding potassium hydroxide to adjust the pH value to 10, keeping the heating temperature and the rotating speed same as those in the step (1), and stirring and cleaning for 8 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating by using II-grade circulating water according to the ratio of 1:10 of the activated carbon to the leacheate for 10 times, feeding the obtained filter cake into an acid washing process, and feeding the filtrate into a water treatment system.
(3) Acid washing process: mixing the activated carbon obtained in the step (2) with II-grade circulating water according to a mass ratio of 1:10, adding hydrochloric acid to adjust the pH to 2, heating in a water bath to 60 ℃, adding mechanical stirring at a rotating speed of 200rpm, and stirring for 8 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching by using II-grade circulating water according to the ratio of 1:10 of the activated carbon to the leacheate, dehydrating until filtrate is neutral, feeding the obtained filter cake into an I-grade water washing process, and feeding the filtrate into a water treatment system.
(4) I-level water washing procedure: mixing the activated carbon after acid washing in the step (3) with deionized water according to the mass ratio of 1:10, heating the mixture in a water bath to 60 ℃, mechanically stirring the mixture for 8 hours at the rotating speed of 200rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating the slurry for 10 times by using the deionized water according to the ratio of the activated carbon to the leaching solution of 1:10, feeding the obtained filter cake into a second-level washing process, and returning the filtrate serving as first-level circulating water to the neutralization process for use.
(5) And II-stage water washing procedure: and (4) mixing the activated carbon subjected to the I-level water washing with deionized water according to the mass ratio of 1:10, heating the mixture in a water bath to 60 ℃, mechanically stirring the mixture for 8 hours at the rotating speed of 200rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching the slurry with deionized water according to the ratio of 1:10 of the activated carbon to leacheate for 10 times to obtain a washed activated carbon finished product, and returning the filtrate serving as II-level circulating water to the acid washing process for use.
And drying the finished product of the activated carbon to obtain the activated carbon for the high-purity super capacitor, wherein the ash content of the activated carbon is 0.04 percent, the iron ion content is 44ppm, the nickel ion content is 4ppm, and the potassium ion content is 80 ppm.
Example 2
Embodiment 2 provides a method for cleaning activated carbon, which specifically comprises the following steps:
(1) a neutralization process, namely mixing 2kg of activated carbon with I-grade circulating water according to a mass ratio of 1:100, adding nitric acid to adjust the pH to 10, heating in a water bath to 65 ℃, adding mechanical stirring at a rotating speed of 100rpm, and stirring for 6 hours to obtain slurry; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating by using I-grade circulating water for 8 times according to the ratio of 1:10 of the activated carbon to the leacheate, allowing the obtained filter cake to enter an alcohol phase alkaline washing process, and allowing the filtrate to enter a water treatment system.
(2) Alcohol phase alkali washing process: mixing the activated carbon obtained in the neutralization step with an ethanol solution with the mass fraction of 60% according to the mass ratio of 1:100, adding nitric acid to adjust the pH to 4, heating in a water bath to 65 ℃, and mechanically stirring for 2 hours at the rotating speed of 100 rpm; adding ammonia water to adjust the pH to 8, keeping the heating temperature and the rotating speed same as those in the step (1), and stirring and cleaning for 6 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating by using II-grade circulating water according to the ratio of 1:10 of the activated carbon to the leacheate for 8 times, feeding the obtained filter cake into an acid washing process, and feeding the filtrate into a water treatment system.
(3) Acid washing process: mixing the activated carbon obtained in the step (2) with II-grade circulating water according to the mass ratio of 1:100, adding nitric acid to adjust the pH to 2, heating in a water bath to 65 ℃, adding mechanical stirring at the rotating speed of 100rpm, and stirring for 6 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching by using II-grade circulating water according to the ratio of 1:10 of the activated carbon to the leacheate, dehydrating until filtrate is neutral, feeding the obtained filter cake into an I-grade water washing process, and feeding the filtrate into a water treatment system.
(4) I-level water washing procedure: mixing the activated carbon after acid washing in the step (3) with deionized water according to the mass ratio of 1:100, heating the mixture in a water bath to 65 ℃, mechanically stirring the mixture for 6 hours at the rotating speed of 100rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating the slurry for 8 times by using the deionized water according to the ratio of the activated carbon to the leacheate of 1:10, feeding the obtained filter cake into a second-level washing process, and returning the filtrate to the neutralization process as first-level circulating water for use.
(5) And II-stage water washing procedure: and (4) mixing the activated carbon subjected to the I-level water washing with deionized water according to the mass ratio of 1:100, heating the mixture in a water bath to 65 ℃, mechanically stirring the mixture for 6 hours at the rotating speed of 100rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching the slurry with deionized water according to the ratio of 1:10 of the activated carbon to leacheate for 8 times to obtain a washed activated carbon finished product, and returning the filtrate serving as II-level circulating water to the acid washing process for use.
And drying the finished product of the activated carbon to obtain the activated carbon for the high-purity super capacitor, wherein the ash content of the activated carbon is 0.05 percent, the iron ion content is 56ppm, the nickel ion content is 6ppm, and the potassium ion content is 86 ppm.
Example 3
Embodiment 3 provides a method for cleaning activated carbon, which specifically comprises the following steps:
(1) a neutralization process, namely mixing 5kg of activated carbon with I-grade circulating water according to a mass ratio of 1:50, adding hydrochloric acid to adjust the pH to 9, heating in a water bath to 80 ℃, adding mechanical stirring at a rotating speed of 500rpm, and stirring for 12h to obtain slurry; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating by using I-grade circulating water for 20 times according to the ratio of 1:20 of the activated carbon to the leacheate, allowing the obtained filter cake to enter an alcohol phase alkaline washing process, and allowing the filtrate to enter a water treatment system.
(2) Alcohol phase alkali washing process: mixing the activated carbon obtained in the neutralization step with an ethanol solution with the mass fraction of 50% according to the mass ratio of 1:50, adding hydrochloric acid to adjust the pH value to 3, heating in a water bath to 80 ℃, and mechanically stirring for 3 hours at the rotating speed of 500 rpm; adding sodium hydroxide to adjust the pH to 11, keeping the heating temperature and the rotating speed same as those in the step (1), and stirring and cleaning for 9 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating by using II-grade circulating water for 20 times according to the ratio of 1:20 of the activated carbon to the leacheate, feeding the obtained filter cake into an acid washing process, and feeding the filtrate into a water treatment system.
(3) Acid washing process: mixing the activated carbon obtained in the step (2) with II-grade circulating water according to the mass ratio of 1:50, adding hydrochloric acid to adjust the pH value to 1, heating in a water bath to 80 ℃, adding mechanical stirring at the rotating speed of 500rpm, and stirring for 12 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching by using II-grade circulating water according to the ratio of 1:20 of the activated carbon to the leacheate, dehydrating until filtrate is neutral, feeding the obtained filter cake into an I-grade water washing process, and feeding the filtrate into a water treatment system.
(4) I-level water washing procedure: and (3) mixing the activated carbon after acid washing with deionized water according to the mass ratio of 1:50, heating in a water bath to 80 ℃, mechanically stirring for 12 hours at the rotating speed of 500rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating with deionized water for 20 times according to the ratio of 1:20 of the activated carbon to the leacheate, feeding the obtained filter cake into a second-stage water washing process, and returning the filtrate serving as first-stage circulating water to the neutralization process for use.
(5) And II-stage water washing procedure: and (4) mixing the activated carbon subjected to the I-level water washing with deionized water according to the mass ratio of 1:50, heating the mixture in a water bath to 80 ℃, mechanically stirring the mixture for 12 hours at the rotating speed of 500rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching the slurry with deionized water according to the ratio of 1:20 of the activated carbon to leacheate for 20 times to obtain a washed activated carbon finished product, and returning the filtrate serving as II-level circulating water to the acid washing process for use.
And drying the finished product of the activated carbon to obtain the activated carbon for the high-purity super capacitor, wherein the ash content of the activated carbon is 0.03 percent, the iron ion content is 26ppm, the nickel ion content is 2ppm, and the potassium ion content is 48 ppm.
Example 4
Embodiment 4 provides a method for cleaning activated carbon, which specifically comprises the following steps:
(1) a neutralization process, namely mixing 1kg of activated carbon with I-grade circulating water according to a mass ratio of 1:5, adding sulfuric acid to adjust the pH value to 10, heating in a water bath to 45 ℃, adding mechanical stirring at a rotating speed of 350rpm, and stirring for 4 hours to obtain slurry; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating by using I-grade circulating water for 15 times according to the ratio of 1:3 of the activated carbon to the leacheate, allowing the obtained filter cake to enter an alcohol phase alkaline washing process, and allowing the filtrate to enter a water treatment system.
(2) An alkali washing process: mixing the activated carbon obtained in the neutralization procedure with deionized water according to the mass ratio of 1:5, adding sulfuric acid to adjust the pH value to 2, heating in a water bath to 45 ℃, and mechanically stirring for 2 hours at the rotating speed of 350 rpm; adding potassium hydroxide to adjust the pH value to 10, keeping the heating temperature and the rotating speed same as those in the step (1), and stirring and cleaning for 2 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating by using II-grade circulating water according to the ratio of 1:3 of the activated carbon to the leacheate for 15 times, feeding the obtained filter cake into an acid washing process, and feeding the filtrate into a water treatment system.
(3) Acid washing process: mixing the activated carbon obtained in the step (2) with II-grade circulating water according to a mass ratio of 1:5, adding sulfuric acid to adjust the pH value to 1, heating in a water bath to 45 ℃, adding mechanical stirring at a rotating speed of 350rpm, and stirring for 4 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching by using II-grade circulating water according to the ratio of 1:3 of the activated carbon to the leacheate, dehydrating until filtrate is neutral, feeding the obtained filter cake into a I-grade water washing process, and feeding the filtrate into a water treatment system.
(4) I-level water washing procedure: mixing the activated carbon after acid washing in the step (3) with deionized water according to the mass ratio of 1:5, heating the mixture in a water bath to 45 ℃, mechanically stirring the mixture for 4 hours at the rotating speed of 350rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating the slurry for 15 times by using the deionized water according to the ratio of the activated carbon to the leacheate of 1:3, feeding the obtained filter cake into a second-level water washing process, and returning the filtrate to the neutralization process as first-level circulating water for use.
(5) And II-stage water washing procedure: and (4) mixing the activated carbon subjected to the I-level water washing with deionized water according to the mass ratio of 1:5, heating the mixture in a water bath to 45 ℃, mechanically stirring the mixture for 4 hours at the rotating speed of 350rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching the slurry with deionized water according to the ratio of the activated carbon to the leacheate of 1:3, dehydrating the slurry for 15 times to obtain a washed activated carbon finished product, and returning the filtrate to the acid washing process as II-level circulating water for use.
And drying the finished product of the activated carbon to obtain the activated carbon for the high-purity super capacitor, wherein the ash content of the activated carbon is 0.05 percent, the iron ion content is 88ppm, the nickel ion content is 10ppm, and the potassium ion content is 96 ppm.
Example 5
Embodiment 5 provides a method for cleaning activated carbon, which specifically comprises the following steps:
(1) a neutralization process, namely mixing 2kg of activated carbon with I-grade circulating water according to a mass ratio of 1:80, adding nitric acid to adjust the pH to 8, heating in a water bath to 70 ℃, adding mechanical stirring at a rotating speed of 230rpm, and stirring for 8 hours to obtain slurry; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating for 5 times by using I-grade circulating water according to the ratio of 1:15 of the activated carbon to the leacheate, allowing the obtained filter cake to enter an alcohol phase alkaline washing process, and allowing the filtrate to enter a water treatment system.
(2) Alcohol phase alkali washing process: mixing the activated carbon obtained in the neutralization step with 20% ethanol solution according to the mass ratio of 1:80, adding nitric acid to adjust the pH to 3, heating in a water bath to 70 ℃, and mechanically stirring for 2 hours at the rotating speed of 230 rpm; adding sodium hydroxide to adjust the pH to 9, keeping the heating temperature and the rotating speed same as those in the step (1), and stirring and cleaning for 6 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating by using II-grade circulating water for 5 times according to the ratio of 1:15 of the activated carbon to the leacheate, feeding the obtained filter cake into an acid washing process, and feeding the filtrate into a water treatment system.
(3) Acid washing process: mixing the activated carbon obtained in the step (2) with II-grade circulating water according to the mass ratio of 1:80, adding hydrochloric acid to adjust the pH value to 2, heating in a water bath to 70 ℃, adding mechanical stirring at the rotating speed of 230rpm, and stirring for 8 hours; and then, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching by using II-grade circulating water according to the ratio of 1:15 of the activated carbon to the leacheate, dehydrating until filtrate is neutral, feeding the obtained filter cake into an I-grade water washing process, and feeding the filtrate into a water treatment system.
(4) I-level water washing procedure: mixing the activated carbon after acid washing in the step (3) with deionized water according to the mass ratio of 1:80, heating the mixture in a water bath to 70 ℃, mechanically stirring the mixture for 8 hours at the rotating speed of 230rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching and dehydrating the slurry for 5 times by using the deionized water according to the ratio of the activated carbon to the leacheate of 1:15, feeding the obtained filter cake into a second-level water washing process, and returning the filtrate serving as first-level circulating water to the neutralization process for use.
(5) And II-stage water washing procedure: and (4) mixing the activated carbon subjected to the I-level water washing with deionized water according to the mass ratio of 1:80, heating the mixture in a water bath to 70 ℃, mechanically stirring the mixture for 8 hours at the rotating speed of 230rpm, pumping the slurry into a filter pressing device for dehydration, repeatedly leaching the slurry with deionized water according to the ratio of 1:15 of the activated carbon to leacheate for 5 times to obtain a washed activated carbon finished product, and returning the filtrate serving as II-level circulating water to the acid washing process for use.
And drying the finished product of the activated carbon to obtain the activated carbon for the high-purity super capacitor, wherein the ash content of the activated carbon is 0.04 percent, the iron ion content is 38ppm, the nickel ion content is 4ppm, and the potassium ion content is 60 ppm.
Comparative example 1
Comparative example 1 provides a method for cleaning activated carbon, and the comparative example 1 is different from example 5 in that reference is made to example 5: in the step (2), the activated carbon obtained in the neutralization procedure is mixed with an ethanol solution, nitric acid is added to adjust the pH value to 5, and the mixture is heated to 95 ℃ in a water bath; adding sodium hydroxide to adjust the pH to 12; the rest is the same as in example 5.
And drying the finished product of the activated carbon to obtain the activated carbon for the high-purity super capacitor, wherein the ash content of the activated carbon is 0.12 percent, the iron ion content is 304ppm, the nickel ion content is 45ppm, and the potassium ion content is 102 ppm.
Comparative example 2
Comparative example 2 provides a method for cleaning activated carbon, and comparative example 2 is different from example 5 in that reference is made to example 5: in the step (2), the activated carbon obtained in the neutralization procedure is mixed with an ethanol solution, nitric acid is added to adjust the pH value to 1, and the mixture is heated to 35 ℃ in a water bath; adding sodium hydroxide to adjust the pH to 6; the rest is the same as in example 5.
And drying the finished product of the activated carbon to obtain the activated carbon for the high-purity super capacitor, wherein the ash content of the activated carbon is 0.09 percent, the iron ion content is 196ppm, the nickel ion content is 65ppm, and the potassium ion content is 204 ppm.
The method adopts a multi-stage cleaning process, and achieves the purpose of separating the active carbon from the metal impurities by utilizing the solubility difference of the impurities of iron ions, nickel ions and potassium ions under different pH values and the selective adsorption of the active carbon on ethanol and the impurity ions; meanwhile, the multi-stage circulating water is repeatedly used, so that the cleaning water is reduced, and the water resource is saved. Test shows that the ash content of the activated carbon cleaned by the method can be reduced to 0.03-0.05%, the iron ion content is 26-88ppm, the nickel ion content is 2-10ppm, the potassium ion content is 48-96ppm, the impurity content is low, and the water is saved by more than 35% compared with the traditional cleaning mode under similar cleaning effect; the method has the advantages of simple and feasible process, high washing efficiency, low energy consumption, low requirement on equipment, capability of greatly reducing the washing cost and good practicability.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (9)
1. A method for cleaning activated carbon, comprising the steps of:
mixing activated carbon to be cleaned with a first acid solution for neutralization reaction, and dehydrating to obtain neutralized activated carbon;
mixing the neutralized activated carbon with a second acid solution, heating to 45-80 ℃, and adjusting the pH value to 2-4 to obtain acidic activated carbon;
mixing the acidic activated carbon with alkali liquor, heating to adjust the pH value to 8-11, and dehydrating to obtain alkali washing activated carbon;
carrying out acid washing and water washing on the alkali washing activated carbon to finish activated carbon cleaning;
mixing the neutralized activated carbon with a second acid solution and heating to 45-80 ℃, including,
mixing the neutralized activated carbon with an alcohol solution and a second acid solution, and heating to 45-80 ℃, wherein the mass ratio of the neutralized activated carbon to the alcohol solution is 0.8-1.2: 5-100.
2. The method for cleaning activated carbon according to claim 1, wherein the alcohol solution is any one of: the methanol solution and the ethanol solution, wherein the mass fraction of the ethanol solution is less than or equal to 60 percent.
3. The method for cleaning activated carbon as claimed in claim 1, wherein the temperature is 45-80 ℃, the stirring speed is 100-500rpm, and the stirring time is 2-12 h; the pH value at the end of the neutralization reaction is 8-10.
4. The method as claimed in claim 1, wherein the acidic activated carbon is heated and stirred during the process of adjusting pH value by mixing with alkali solution, the heating temperature is 45-80 ℃, the stirring speed is 100-500rpm, and the stirring time is 2-12 h.
5. The method for cleaning activated carbon according to claim 1, wherein the first acid solution is at least one of: hydrochloric acid, sulfuric acid and nitric acid, wherein the second acid solution is at least one of the following acids: hydrochloric acid, sulfuric acid, nitric acid.
6. The method for cleaning activated carbon according to claim 1, wherein the alkali solution is at least one of: potassium hydroxide, sodium hydroxide and ammonia water.
7. The method for cleaning activated carbon according to claim 1, wherein the acid washing is performed by mixing the alkali-washed activated carbon with water and adjusting the pH to 1-2 with an acid solution.
8. The method for cleaning activated carbon according to claim 1, wherein the water washing is to mix deionized water with activated carbon, heat and stir, then dehydrate, and repeatedly rinse and dehydrate with deionized water; the heating temperature is 45-80 ℃, the stirring speed is 100-500rpm, and the stirring time is 2-12 h.
9. The method of claim 8, wherein the deionized water is water having an electrical resistivity of 0.5-10M Ω.
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| JP2008207982A (en) * | 2007-02-26 | 2008-09-11 | Kansai Coke & Chem Co Ltd | Method of highly purifying activated carbon |
| JP2008303083A (en) * | 2007-06-05 | 2008-12-18 | Kansai Coke & Chem Co Ltd | Method for highly purifying activated carbon |
| CN102502621A (en) * | 2011-11-28 | 2012-06-20 | 中南大学 | Post-treatment process for preparing super-capacitor active carbon with super-low ash content |
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| JP2008207982A (en) * | 2007-02-26 | 2008-09-11 | Kansai Coke & Chem Co Ltd | Method of highly purifying activated carbon |
| JP2008303083A (en) * | 2007-06-05 | 2008-12-18 | Kansai Coke & Chem Co Ltd | Method for highly purifying activated carbon |
| CN102502621A (en) * | 2011-11-28 | 2012-06-20 | 中南大学 | Post-treatment process for preparing super-capacitor active carbon with super-low ash content |
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