CN104118875B - A kind of ultracapacitor activated carbon cleaning method and special purpose device thereof - Google Patents
A kind of ultracapacitor activated carbon cleaning method and special purpose device thereof Download PDFInfo
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- CN104118875B CN104118875B CN201410368512.3A CN201410368512A CN104118875B CN 104118875 B CN104118875 B CN 104118875B CN 201410368512 A CN201410368512 A CN 201410368512A CN 104118875 B CN104118875 B CN 104118875B
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Abstract
The invention discloses a kind of ultracapacitor activated carbon cleaning method and special purpose device thereof, the hydrochloric acid solution dipping of the activated carbon 15wt% that the method is learnt from else's experience pretreated, hydrochloric acid solution is boiled 30 90min by the steam being passed through 0.1 0.5MPa, static 15 hours, being passed through steam washing with deionized water more neutral, the tenor in gained activated carbon is reduced to below 200ppm.The ultracapacitor activated carbon cleaning method of the present invention, find through great many of experiments, combine the control to activated carbon particle size with steam, utilize the strength penetration of steam, repeatedly impregnate washing by acid and deionized water, content of beary metal in activated carbon can be substantially reduced.Our experiments show that, activated carbon tenor can be made to drop to below 200ppm by the method, washing process adds oxalic acid (metal chelating agent), content of beary metal can be made to be down to below 100ppm, there is good practicality.
Description
Technical field
The invention belongs to supercapacitor technologies field, be specifically related to a kind of ultracapacitor activated carbon cleaning method and special purpose device thereof.
Background technology
Activated carbon with the aperture structure of its prosperity and stable physicochemical property extensive application in terms of electrode material for super capacitor, is the most suitably used material of current electrode of super capacitor.But, in order to improve the specific surface area of activated carbon and the control to its aperture structure, the general mode using alkali and steam activation manufactures.Steam activation needs at high temperature to carry out, and steam is higher to the degree of purity of prepared product as activator, and the activated carbon specific surface area that its shortcoming is obtained is not easy to improve, thus causes obtained electrode material gram volume the highest.The obtained activated carbon of alkali activation, with alkali as activator, its advantage is that obtained activated carbon specific surface area is big, and technique is simple.But a disadvantage is that a large amount of activator remains in activated carbon, the later stage needs to carry out substantial amounts of cleaning.At high temperature there is due to alkali the strongest corrosivity, whole activation body of heater is also had a certain degree of corrosiveness.In rustless steel activation furnace, some beavy metal impurities can be introduced in activated carbon, therefore the activated carbon produced does not contains only substantial amounts of residual alkali activator, also has some beavy metal impurities.These metal impurities can occur chemical reaction, even some metal impurities to be restored during ultracapacitor discharge and recharge, causes capacitor short-circuit, largely effects on the life-span of ultracapacitor.
In order to remove these metal impurities, the method that general commonly used acid solution dipping cleans.But a lot of metal impurities are coated on inside activated carbon, simple acid solution dipping is difficult to dissolve away, and these metal impurities also can increase the self discharge degree of ultracapacitor, increases leakage current, reduces efficiency for charge-discharge.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, it is an object of the invention to provide a kind of ultracapacitor activated carbon cleaning method, makes activated carbon tenor drop to below 200ppm.It is a further object of the present invention to provide the special purpose device of a kind of above-mentioned ultracapacitor activated carbon cleaning method, there is automaticity high, simple to operate, the feature such as the shortest.
Technical scheme: in order to realize foregoing invention purpose, the technical solution used in the present invention is as follows:
A kind of ultracapacitor activated carbon cleaning method, the hydrochloric acid solution dipping of the activated carbon 15wt% learning from else's experience pretreated, hydrochloric acid solution is boiled 30-90min by the steam being passed through 0.1-0.5MPa, static 1-5 hour, being passed through steam washing with deionized water more neutral, the tenor in gained activated carbon is reduced to below 200ppm.
Described ultracapacitor activated carbon cleaning method, is the most first crushed to pretreated activated carbon more than 1000 mesh, then impregnates 1-5 hour with the hydrochloric acid solution of 15wt%.Preferably: in the hydrochloric acid solution of 15wt%, add the oxalic acid solution of 0.5wt%.
Described ultracapacitor activated carbon cleaning method, preferably: with the hydrochloric acid solution of 15wt% dipping, is passed through the steam of 0.1-0.5MPa and hydrochloric acid solution boils 30-90min, static 1-5 hour.Preferably: in the hydrochloric acid solution of 15wt%, add the oxalic acid solution of 0.5wt%.
Described ultracapacitor activated carbon cleaning method, described pretreatment operation is: use deionized water Immesion active carbon, and the steam being passed through 0.3MPa makes it seethe with excitement, cyclic washing, removes most residual activator.Raw material is after alkali activates, containing substantial amounts of residual activator in the activated carbon of production, and the metal impurities being corroded on body of heater, with deionized water dipping, the steam being passed through 0.3MPa makes it seethe with excitement, cyclic washing, and most residual activator is removed.But also some metal impurities being coated in activated carbon and activator also remain on the activated carbon, it is impossible to remove.
The special purpose device of a kind of described ultracapacitor activated carbon cleaning method, including water making device, steam evaporator, draining tank, surge tank, neutralizing tank and vacuum pump；Described water making device is connected with steam evaporator and draining tank respectively by pipeline.Described steam evaporator is connected bottom draining tank by several pipelines, and each pipeline is in being distributed clockwise or counterclockwise；Described draining tank is connected with surge tank, and surge tank top is connected with vacuum pump；Described surge tank connects with neutralizing tank.
Described neutralizing tank includes 3, respectively for filling the tank of sour water, for filling the tank of aqueous alkali, and for being allowed to neutralize into neutrality to reach the tank of emission request with the consumption of aqueous alkali by regulation sour water.
Described steam evaporator by with 3 Thermostable flexible hoses in being distributed in bottom draining tank clockwise or counterclockwise, when steam evaporator is opened, air-flow is in flowing clockwise or counterclockwise, makes the material in draining tank in forming swirl shape clockwise or counterclockwise.
Set polypropylene filter bag at described draining tank, and fit with draining tank.
Beneficial effect: compared with prior art, the ultracapacitor activated carbon cleaning method of the present invention and special purpose device thereof, find through great many of experiments, the control to activated carbon particle size is combined with steam, utilize the strength penetration of steam, repeatedly impregnate washing by acid and deionized water, content of beary metal in activated carbon can be substantially reduced.Our experiments show that, activated carbon tenor can be made to drop to below 200ppm by the method, washing process adds oxalic acid (metal chelating agent), content of beary metal can be made to be down to below 100ppm, there is good practicality.
Accompanying drawing explanation
Fig. 1 is the structural representation that ultracapacitor activated carbon powder cleans device.
Detailed description of the invention
The present invention is described further with specific embodiment below in conjunction with the accompanying drawings.
As it is shown in figure 1, the special purpose device of ultracapacitor activated carbon cleaning method, mainly it is made up of water making device 1, steam evaporator 2, draining tank 3, surge tank 4, neutralizing tank 5, these parts of vacuum pump 6.On draining tank 3, first put into the polypropylene filter bag of 2000 mesh, be allowed to fit with draining tank, then material is put in filter bag.Being made deionization moisture two-way by water making device 1, a-road-through enters steam evaporator 2 and makes steam, and another road is passed through draining tank 3 for cleaning active powdered carbon.Steam evaporator 2 is that clockwise or counterclockwise is distributed in bottom draining tank with 3 high temperature resistant tetrafluoro flexible pipes, steam pressure can arbitrarily regulate from 0.1MPa-0.7MPa as required, when steam evaporator 2 is opened, air-flow is in flowing clockwise or counterclockwise, make the material in draining tank in forming swirl shape clockwise or counterclockwise, make material be sufficiently stirred for and can reach heats.The water that steam boils in draining tank continues for some time, and closes steam, and by 6 water suction surge tanks 4 of vacuum pump, material is then deposited on bottom filter bag in filter cake shape.Opening surge tank 4 bottom valve to be passed into the neutralizing tank 5(of correspondence according to Acidity of Aikalinity and have 3,1 is used for filling sour water, and one is used for filling aqueous alkali, and 1 is neutral to reach emission request for being allowed to the consumption of aqueous alkali to neutralize into by regulation sour water) neutralize.Final needs is washed till neutrality activated carbon powder, repeat the above steps as required.
The package unit various piece of this special purpose device belongs to mature equipment, and automaticity is high, and operator only need to control each motor push button and i.e. can reach preferable cleaning performance.Automaticity is high, simple to operate, the shortest, dipping and sucking filtration carry out in a treatment trough, it is not necessary to material shift, use 0.3-0.5MPa steam be passed through bubbling in groove seethe reach stirring and heating purpose, will not produce any dead angle, product quality is easily controlled.Meanwhile, each several part equipment all belongs to mature equipment, all can automatically control, and equipment cost is low, and whole cleaning process only needs operator, and cost of labor is saved.Operation is simple, and whole cleaning process will not have any loss to material, considerably increases its cleaning efficiency.Clean the neutralized device of sewage after material and reach emission request, environmental protection and energy saving.
Following example are based on this device and carry out.
Embodiment 1
A kind of ultracapacitor activated carbon cleaning method, with petroleum coke for raw material through 500 DEG C of carbonizations 1 hour, products therefrom with charcoal alkali than 1:2 activate in 800 DEG C 2 little time, it is cooled to less than 100 DEG C, with deionized water dipping, the steam being passed through 0.3MPa makes it seethe with excitement, sucking filtration while hot, cyclic washing three times (slightly washing).Take 1kg and slightly wash sample, impregnate with the hydrochloric acid solution 10kg of 15wt%, be passed through the steam of 0.3MPa and hydrochloric acid solution is boiled 30min, static 1-5 hour, then it is passed through steam washing to neutral with deionized water, sucking filtration is dried.The content of beary metal of gained activated carbon is shown in Table 1, it can be seen that after cleaning by the method, and activated carbon total metal content is less than 200ppm.
Embodiment 2
A kind of ultracapacitor activated carbon cleaning method, is crushed to 1000 mesh with slightly washing sample in embodiment 1, takes 1kg, impregnates 1-5 hour with the hydrochloric acid solution 10kg of 15wt%, then is washed with deionized to neutrality, and sucking filtration is dried.The content of beary metal of gained activated carbon is shown in Table 1, it can be seen that after cleaning by the method, and activated carbon total metal content is less than 200ppm.
Embodiment 3
A kind of ultracapacitor activated carbon cleaning method, in Example 1,1kg slightly washes sample, impregnate with the mixed solution of hydrochloric acid 8kg and the 0.5wt% oxalic acid 2kg of 15wt%, operate equally with embodiment 1, the content of beary metal of gained activated carbon is shown in Table 1, can be seen that, after cleaning by the method, activated carbon total metal content is less than 200ppm, and better than the cleaning performance of embodiment 1.
Embodiment 4
A kind of ultracapacitor activated carbon cleaning method, it is crushed to 1200 mesh with embodiment 1 is slightly washed sample, take 1kg, impregnate with the mixed solution of hydrochloric acid 9kg and the 0.5wt% oxalic acid 1kg of 15wt%, operating equally with embodiment 2, the content of beary metal of gained activated carbon is shown in Table 1, it can be seen that after cleaning by the method, activated carbon total metal content is less than 200ppm, and better than the cleaning performance of embodiment 2.
Embodiment 5
A kind of ultracapacitor activated carbon cleaning method, it is crushed to 1300 mesh with embodiment 1 is slightly washed sample, take 1kg, operate equally with embodiment 1, the content of beary metal of gained activated carbon is shown in Table 1, can be seen that, after cleaning by the method, activated carbon total metal content is less than 100ppm, and will be good than the cleaning performance of embodiment 1,2.
Embodiment 6
A kind of ultracapacitor activated carbon cleaning method, it is crushed to 1000 mesh with embodiment 1 is slightly washed sample, take 1kg, impregnate with the mixed solution of hydrochloric acid 9.5kg and the 0.5wt% oxalic acid 0.5kg of 15wt%, operating equally with embodiment 1, the content of beary metal of gained activated carbon is shown in Table 1, it can be seen that after cleaning by the method, activated carbon total metal content is less than 100ppm, and will be good than the cleaning performance of embodiment 1,2,5.
Embodiment 7
A kind of ultracapacitor activated carbon cleaning method, slightly washes sample 1kg in Example 1, impregnate 1-5 hour with the hydrochloric acid solution 10kg of 15wt%, then be washed with deionized to neutrality, and sucking filtration is dried.The content of beary metal of gained activated carbon is shown in Table 1, it can be seen that after cleaning by the method, and activated carbon total metal content is higher than 1000ppm.Illustrating that general pickling effect is less desirable, some beavy metal impurities do not have dissolution.
Beavy metal impurity content in table 1 various embodiments of the present invention activated carbon
| Fe(ppm) | Cr(ppm) | Ni(ppm) | Total amount (ppm) | |
| Embodiment 1 | 71 | 65 | 35 | 171 |
| Embodiment 2 | 89 | 71 | 38 | 198 |
| Embodiment 3 | 46 | 35 | 34 | 115 |
| Embodiment 4 | 55 | 45 | 35 | 135 |
| Embodiment 5 | 34 | 26 | 30 | 90 |
| Embodiment 6 | 24 | 20 | 17 | 61 |
| Embodiment 7 | 451 | 423 | 318 | 1192 |
The result of summary embodiment, in cleaning process, utilizes steam and the control of broken particle diameter, and tenor in activated carbon can be made substantially to reduce, and when adding oxalic acid chelating agent, its cleaning performance is more preferably.Needing strict its metals content impurity that controls for ultracapacitor activated carbon, employing embodiment 6 can reach optimum efficiency.
Claims (3)
1. a ultracapacitor activated carbon cleaning method, it is characterised in that: first pretreated activated carbon is crushed to 1000 mesh with
On, then impregnate 1-5 hour with the hydrochloric acid solution of 15wt%, hydrochloric acid solution is boiled 30-by the steam being passed through 0.1-0.5MPa
90min, static 1-5 hour, then it is passed through the steam washing tenor reduction to neutral, in gained activated carbon with deionized water
To below 200ppm；Wherein, in the hydrochloric acid solution of 15wt%, add the oxalic acid solution of 0.5wt%.
Ultracapacitor activated carbon cleaning method the most according to claim 1, it is characterised in that: described pretreatment operation
For: using deionized water Immesion active carbon, the steam being passed through 0.3MPa makes it seethe with excitement, cyclic washing, removes most residual
Stay activator.
3. the special purpose device of the ultracapacitor activated carbon cleaning method described in a claim 1, it is characterised in that: include that controlling the water circulation sets
Standby (1), steam evaporator (2), draining tank (3), surge tank (4), neutralizing tank (5) and vacuum pump (6)；Described
Water making device (1) be connected with steam evaporator (2) and draining tank (3) respectively by pipeline；Described steam is sent out
Raw device (2) connects draining tank (3) bottom by several pipelines, and each pipeline is in being distributed clockwise or counterclockwise；Described
Draining tank (3) is connected with surge tank (4), and surge tank (4) top is connected with vacuum pump (6)；Described surge tank
(4) connect with neutralizing tank (5)；Described neutralizing tank includes 3, is respectively the tank for filling sour water, for filling aqueous alkali
Tank, and for being allowed to neutralize into neutrality to reach the tank of emission request with the consumption of aqueous alkali by regulation sour water；Described water steams
Gas generator (2) by with 3 Thermostable flexible hoses in be distributed in clockwise or counterclockwise draining tank (3) bottom, work as water
When steam generator is opened, air-flow is in flowing clockwise or counterclockwise, makes the material in draining tank in side clockwise or counterclockwise
To forming swirl shape.
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| CN104787759B (en) * | 2015-04-20 | 2017-09-15 | 德阳烯碳科技有限公司 | A kind of impurity-removing method in graphene preparation process |
| CN104787758B (en) * | 2015-04-20 | 2017-05-03 | 德阳烯碳科技有限公司 | Method for preparing graphene on large scale |
| CN106692081B (en) * | 2016-12-30 | 2019-09-13 | 广东健信制药股份有限公司 | A kind of freeze-dried powder injection of pantoprazole sodium and preparation method |
| CN110117012B (en) * | 2019-05-14 | 2022-09-23 | 江苏哈特尔碳材料科技有限公司 | Granular activated carbon washing equipment |
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| CN102020273A (en) * | 2010-12-09 | 2011-04-20 | 山西新华化工有限责任公司 | Preparation method of coal activated carbon for refinement of monosodium glutamate |
| CN103121680A (en) * | 2013-01-28 | 2013-05-29 | 江苏国正新材料科技有限公司 | Preparation method of ultrahigh-stored energy electrical carbon material |
| CN203998961U (en) * | 2014-07-30 | 2014-12-10 | 江苏捷峰高科能源材料股份有限公司 | A kind of ultracapacitor activity charcoal powder washing unit |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020273A (en) * | 2010-12-09 | 2011-04-20 | 山西新华化工有限责任公司 | Preparation method of coal activated carbon for refinement of monosodium glutamate |
| CN103121680A (en) * | 2013-01-28 | 2013-05-29 | 江苏国正新材料科技有限公司 | Preparation method of ultrahigh-stored energy electrical carbon material |
| CN203998961U (en) * | 2014-07-30 | 2014-12-10 | 江苏捷峰高科能源材料股份有限公司 | A kind of ultracapacitor activity charcoal powder washing unit |
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Effective date of registration: 20200709 Address after: Room 1601, No. 1699, Zuchongzhi South Road, high tech Zone, Kunshan City, Suzhou City, Jiangsu Province Patentee after: Kunshan Kunpeng Lijie polymer material technology Co., Ltd Address before: Qixia District of Nanjing City, Jiangsu province 210000 Gan Jia Bian East 108 Hong Kong Science Park 4 Building 8 layer Patentee before: JIANGSU JF ADVANCED TECHNOLOGIES, Inc. |