CN106252100B - The pretreatment unit and its preprocess method of electrode for super capacitor active material - Google Patents
The pretreatment unit and its preprocess method of electrode for super capacitor active material Download PDFInfo
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- 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
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Abstract
The present invention relates to the pretreatment units and its preprocess method of a kind of electrode for super capacitor active material, belong to technical field of new energy storage.The pretreatment unit includes reaction pile, vacuum pump, charge-discharge test instrument, water bath with thermostatic control, topping-up pump and blender；The preprocess method can it is high with the existing electrode for super capacitor surface of active material functional group content of effective solution, to produce gas serious so that the problems such as monomer capacity is low, internal resistance is big and cycle life is poor for battery core after aging, to obtain, a kind of low surface functional group content, monomer does not play drum, high capacity, low internal resistance and the electrode for super capacitor active material having extended cycle life after aging or high-temperature load.
Description
Technical field
Electrode active is carried out the present invention relates to the pretreatment unit of electrode for super capacitor active material and using the device
The method of property pretreatment.
Background technique
Commercial electrode for super capacitor surface of active material is usually enriched with more active function groups, especially with chemistry
The electrode active material of activation method preparation.If the electrode active material containing more active function groups is prepared into electrode to go forward side by side
One step is assembled into supercapacitor monomer, as long as the monomer assembled is tested through aging or high-temperature load, electrode active material table
The active function groups in face will generate irreversible reaction with electrolyte, generate various mixed gases and cause the active material on electrode
Rapid degradation occurs for layer, so that supercapacitor monomer has been shown as afterwards after tested, drum is serious, capacity reduces, internal resistance increases and the longevity
The Multiple Failure Modes such as life reduction.
The failure modes such as drum can occur after aging or high-temperature load test for supercapacitor monomer, in recent years state
It is inside and outside successively to report a series of solutions.As Chinese patent CN102543481 B report it is a kind of to entering the battery core before shell
The technique of preparatory energization aging techniques assembling supercapacitor monomer.According to the monomer packaging technology that the patent provides, exist first
The battery core of winding is dried in vacuo 8-72 hours at 100-150 DEG C；Then by the battery core of vacuum impregnation organic electrolyte 50
With 2.7V constant pressure energization 10 hours at DEG C；The battery core after energization aging is placed in round aluminum hull again, is finally sealed.But it should
Technical solution is in energization ageing process, and with electrolyte irreversible reaction can occur for more active function groups on electrode, generates
Various mixed gases be discharged from electrolyte, although be able to extend monomer has occurred the bulging time during follow-up test,
But since electrode has been deteriorated in ageing process, it is insufficient to still result in monomer cycle life.Kiyoshi Horita etc. exists
[J] .Carbon, 1996,34 (2) propose the surface state by modification carbon black in 217-222, by the functional group of black carbon surface
Hydrophily is changed by hydrophobicity, the carbon black containing hydrophilic functional group is easy to stir into slurry in water, but either dredges
Water functional group or hydrophilic functional groups all can occur irreversible reaction with electrolyte in supercapacitor ageing process, cause
Monomer plays the Multiple Failure Modes such as drum.
Summary of the invention
For above-mentioned supercapacitor in the prior art, generation monomer drum is serious after aging or high-temperature load test, holds
The Multiple Failure Modes such as amount reduces, internal resistance increases and the service life is reduced, applicant proposed the agings by simulation supercapacitor
Electrode for super capacitor active material is placed in the reaction pile of pretreatment unit and leads to by technique autonomous Design pretreatment unit
It is electro-active, the technical solution of the excessive active function groups on electrode active material surface is removed to the maximum extent.
The first aspect of the present invention provides a kind of electrode for super capacitor active material pretreatment unit, described device
Including reaction pile, vacuum pump, charge-discharge test instrument, water bath with thermostatic control, topping-up pump and blender, wherein react the outside of pile
Internal to be divided into positive pole zone and negative regions by intermediate diaphragm for insulating layer, plus plate current-collecting body is located in reaction pile just
In polar region domain, negative current collector is located in the negative regions in reaction pile, reacts the positive pole zone in pile and negative regions
Respectively it is furnished with a blender, reacts interface there are two the tops of pile, be connected respectively with topping-up pump and vacuum pump；The reaction electricity
Heap plus plate current-collecting body passes through insulating layer through lead-out wire and is connected with the positive terminal of charge-discharge test instrument, reacts pile negative pole currect collecting
Body passes through insulating layer through lead-out wire and is connected with the negative terminal of charge-discharge test instrument；The reaction pile is placed in water bath with thermostatic control
In.
In some embodiments, the volume of the reaction pile is 10L, and top can freely open, in order to reaction
Electrode for super capacitor active material is added in the positive pole zone of pile and negative regions；Positioned at reaction pile positive pole zone
The electrode active material in the region and supercapacitor can be stirred into uniform slurry with electrolyte by blender, be located at reaction
The blender of pile negative regions can stir into the electrode active material in the region and supercapacitor uniformly with electrolyte
Slurry；It will react at the top of pile after sealing, and vacuum degree≤- 0.098Mpa can be evacuated to by pile is reacted with vacuum pump；
The topping-up pump can be to reaction pile quantification fluid injection；The water bath with thermostatic control controllable temperature range is 5 DEG C -100 DEG C, temperature control essence
Degree is ± 0.1 DEG C.
The second aspect of the present invention provides a kind of pretreated method of electrode for super capacitor active material, the side
Method uses aforementioned pretreatment unit comprising following steps:
1) electrode for super capacitor active material is separately added into the positive pole zone and negative regions of reaction pile, it is close
Envelope reaction pile is betted in vacuum degree≤- 0.098Mpa into super electrolyte for capacitor, coordination electrode active material and electrolysis
Liquid forms the slurry that range of solid content is 10wt%-50wt%；
2) temperature of regulating thermostatic water-bath connects the anode collection of reaction pile with charge-discharge test instrument to 60 DEG C -80 DEG C
Body and negative current collector, first by reaction pile constant-current charge to 2.5V-3.0V, then to reaction pile constant pressure at 2.5V-3.0V
Charging 8 hours or more, pile will be reacted after charging complete and is discharged to 0.1V hereinafter, completing the aging of slurry；
3) slurry after aging is taken out from from reaction pile, it is dilute with solvent that is identical as electrolyte composition or can mixing
Slurry is released, is washed out and obtained by drying to pretreatment electrode active material.
In some embodiments, the electrode active material is selected from active carbon, graphene, activated carbon fibre, charcoal gas
Gel or carbon nanotube.
In some embodiments, the plus plate current-collecting body or the negative current collector are selected from aluminium, copper, silver, Jin Huo
Metal mesh or metal plate made of platinum.
In some embodiments, the reaction pile diaphragm is selected from cellulosic separator, polyethylene diagrams or poly- third
Alkene diaphragm.
In some embodiments, the acetonitrile that the supercapacitor is selected from tetraethyl ammonium tetrafluoro boric acid with electrolyte is molten
Liquid, the carbonic allyl ester solution of tetraethyl ammonium tetrafluoro boric acid, the acetonitrile solution of triethylmethylammonium tetrafluoro boric acid, triethyl methyl
The carbonic allyl ester solution of ammonium tetrafluoro boric acid, the SP2 type high-voltage electrolyte of SK group, South Korea and the DLC3702 type of company, Xin Zhou nation
One of high-voltage electrolyte；Electrolyte choosing concentration be can be 0.7M-2.5M.In some embodiments, electrolyte is dense
Degree is 1M.
In some embodiments, it dilutes electrode active material slurry or the new electrode active material of cleaning and is selected from second with solvent
Nitrile, propene carbonate, chloroform, carbon tetrachloride, benzene, normal propyl alcohol, isopropanol, acrylonitrile, ethyl acetate, dichloroethanes, ethyl alcohol, second
One of ether or carbon disulfide are a variety of.
Water used in embodiments of the present invention is deionized water.
" room temperature " of the present invention indicates 20-30 DEG C of temperature.
The definition "or" that the present invention uses indicates that alternative can combine them if applicable, that is,
It says, term "or" includes each listed independent alternative and their combination.For example, " solvent is selected from acetonitrile, carbonic acid
Acrylic ester, chloroform, carbon tetrachloride, benzene, normal propyl alcohol, isopropanol, acrylonitrile, ethyl acetate, dichloroethanes, ethyl alcohol, ether or two
Nitric sulfid." indicate solvent can be acetonitrile, propene carbonate, chloroform, carbon tetrachloride, benzene, normal propyl alcohol, isopropanol, acrylonitrile,
It is ethyl acetate, dichloroethanes, ethyl alcohol, ether, one or more among carbon disulfide.
Unless explicitly stated otherwise in contrast, otherwise, all ranges that the present invention quotes include end value.For example, " 60-80
Water-bath at DEG C " indicates that the range of bath temperature T is 60 DEG C≤T≤80 DEG C.
Technical solution of the present invention can be with effective solution existing electrode for super capacitor surface of active material functional group
Content is high, to produce gas serious so that the problems such as monomer capacity is low, internal resistance is big and cycle life is poor for battery core after aging, to obtain one
The low surface functional group content of kind, monomer does not play drum, high capacity, low internal resistance and has extended cycle life super after aging or high-temperature load
Grade capacitor electrode active material.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the pretreatment unit of electrode for super capacitor active material.
In Fig. 1,1 is reaction pile；2 be vacuum pump；3 be charge-discharge test instrument；4 be water bath with thermostatic control；5 be topping-up pump；6 are
Blender；7 be reaction pile plus plate current-collecting body；8 be reaction pile negative current collector；9 be diaphragm；10 be cushion block.
Specific embodiment
As described below is the preferred embodiment of the present invention, and what the present invention was protected is not limited to following preferred implementation side
Formula.It should be pointed out that for those skilled in the art on the basis of the inventive concept, several deformations for making and
It improves, belongs to protection scope of the present invention.Raw material used in embodiment can be obtained through commercial channels.
Embodiment 1
1000 grams of activated carbon for super capacitors are weighed to be separately added into the positive pole zone and negative regions of reaction pile, it is close
Envelope reaction pile is evacuated to -0.098MPa for pile is reacted with vacuum pump；2000 grams are injected into reaction pile with topping-up pump
Solution of the 1M tetraethyl ammonium tetrafluoro boric acid in acetonitrile is stirred to react positive pole zone and the cathode area of pile with blender respectively
Domain makes the solution of activated carbon for super capacitors and 1M tetraethyl ammonium tetrafluoro boric acid in acetonitrile form solid content 33.3wt%
Slurry；The temperature of regulating thermostatic water-bath is to 60 DEG C, after reacting stack temperature and reaching stable, is connected with charge-discharge test instrument anti-
The plus plate current-collecting body and negative current collector of pile are answered, first by reaction pile constant-current charge to 2.7V, then to reaction electricity at 2.7V
Heap constant-voltage charge 10 hours, reaction pile is discharged to 0V after charging complete；Slurry after aging is taken from from reaction pile
Out, it with 2000 grams of dilution in acetonitrile slurries, filters, obtains pretreatment activated carbon for super capacitors；Supercapacitor will be pre-processed
It is cleaned 3 times with active carbon with 3000 grams of acetonitriles, is dried at 120 DEG C.
The dry Pre-Treatment of Activated material of gained is successively obtained into the electrode with a thickness of 200 μm after slurrying, coating, roll-in.
Electrode is cut into wide 35mm, positive length 570mm, cathode length 525mm.The super capacitor produced using Japanese NKK company
The dedicated TF4035 type diaphragm of device is wound into battery core together with the positive and negative anodes cut.60 battery cores are taken to be placed in 1M tetraethyl ammonium tetrafluoro
Vacuum impregnation is to saturation imbibition state in the solution in acetonitrile for boric acid, and by impregnated battery core loading shell, sealing obtains Φ
22*45 welding needle type supercapacitor monomer.Take 30 monomers at 60 DEG C with 2.7V constant pressure energization 1000 hours, observation monomer is
It is no that drum, the capacity of test unit and internal resistance has occurred.Remaining monomer is first with 5A constant-current charge to 2.7V, then with 5A constant-current discharge
It to 1.35V, and is recycled 100,000 times by this charge and discharge electric condition, whether observation monomer has occurred drum, the capacity and direct current of test unit
Internal resistance.Test result is shown in Table 1.
Embodiment 2
It weighs 1000 grams of graphenes to be separately added into the positive pole zone and negative regions of reaction pile, sealing reaction pile,
- 0.098MPa is evacuated to by pile is reacted with vacuum pump；1500 grams of 1M tetraethyl ammoniums are injected into reaction pile with topping-up pump
Solution of the tetrafluoro boric acid in propene carbonate is stirred to react positive pole zone and the negative regions of pile with blender respectively, makes
The solution of graphene and 1M tetraethyl ammonium tetrafluoro boric acid in propene carbonate forms the slurry that solid content is 40wt%；It adjusts permanent
After reacting stack temperature and reaching stable, the anode of reaction pile is connected with charge-discharge test instrument to 70 DEG C for the temperature of tepidarium
Collector and negative current collector, first by reaction pile constant-current charge to 2.5V, then to reaction pile constant-voltage charge 10 at 2.5V
Hour, reaction pile is discharged to 0V after charging complete；Slurry after aging is taken out from from reaction pile, with 3000 grams of carbon
Acid propylene ester diluted slurry, filtering, obtains pretreating graphite alkene；Pretreating graphite alkene is cleaned 3 with 2000 grams of propene carbonates
It is secondary, it is dried at 180 DEG C.
With embodiment 1, test result is shown in Table 1 for electrode preparation, monomer assembling and test item.
Embodiment 3
It weighs 1000 grams of activated carbon fibre to be separately added into the positive pole zone and negative regions of reaction pile, sealing reaction electricity
Heap is evacuated to -0.098MPa for pile is reacted with vacuum pump；3000 grams of 1M triethyl groups are injected into reaction pile with topping-up pump
Solution of the methyl ammonium tetrafluoro boric acid in propene carbonate is stirred to react positive pole zone and the cathode area of pile with blender respectively
Domain makes activated carbon fibre and 1M triethylmethylammonium tetrafluoro boric acid form solid content in the solution in propene carbonate
The slurry of 25wt%；The temperature of regulating thermostatic water-bath is to 70 DEG C, after reacting stack temperature and reaching stable, with charge-discharge test instrument
The plus plate current-collecting body and negative current collector of connection reaction pile, first will reaction pile constant-current charge it is right to 2.5V, then at 2.5V
Reaction pile is discharged to 0V after charging complete by reaction pile constant-voltage charge 10 hours；By the slurry after aging from from reaction electricity
It is taken out in heap, with 2000 grams of ethyl alcohol diluted slurries, filtering obtains Pre-Treatment of Activated Carbon fibe；By Pre-Treatment of Activated Carbon fiber Wesy
2500 grams of ethyl alcohol clean 3 times, dry at 150 DEG C.
With embodiment 1, test result is shown in Table 1 for electrode preparation, monomer assembling and test item.
Embodiment 4
It weighs 1000 grams of charcoal-aero gels to be separately added into the positive pole zone and negative regions of reaction pile, sealing reaction electricity
Heap is evacuated to -0.098MPa for pile is reacted with vacuum pump；1200 grams of 1M triethyl groups are injected into reaction pile with topping-up pump
Solution of the methyl ammonium tetrafluoro boric acid in acetonitrile is stirred to react positive pole zone and the negative regions of pile with blender respectively, makes
The solution of charcoal-aero gel and 1M triethylmethylammonium tetrafluoro boric acid in acetonitrile forms the slurry that solid content is 45.5wt%；It adjusts
The temperature of water bath with thermostatic control is to 60 DEG C, after reacting stack temperature and reaching stable, is connecting reaction pile just with charge-discharge test instrument
Pole collector and negative current collector, first by reaction pile constant-current charge to 2.7V, then to reaction pile constant-voltage charge at 2.7V
10 hours, reaction pile is discharged to 0V after charging complete；Slurry after aging is taken out from from reaction pile, with 3500 grams
Ethyl acetate diluted slurry, filtering obtain pretreatment charcoal-aero gel；Pretreatment charcoal-aero gel is cleaned with 2500 grams of ethyl acetate
It 3 times, is dried at 100 DEG C.
With embodiment 1, test result is shown in Table 1 for electrode preparation, monomer assembling and test item.
Embodiment 5
It weighs 1000 grams of carbon nanotubes to be separately added into the positive pole zone and negative regions of reaction pile, sealing reaction electricity
Heap is evacuated to -0.098MPa for pile is reacted with vacuum pump；4000 Ke Xin cosmos nations public affairs are injected into reaction pile with topping-up pump
The DLC3702 type high-voltage electrolyte of department, is stirred to react positive pole zone and the negative regions of pile with blender respectively, makes carbon nanometer
The DLC3702 type high-voltage electrolyte of Guan Yuxin Zhou Bang company forms the slurry that solid content is 20wt%；The temperature of regulating thermostatic water-bath
It spends to 60 DEG C, after reacting stack temperature and reaching stable, connects the plus plate current-collecting body of reaction pile with charge-discharge test instrument and bear
Pole collector, first by reaction pile constant-current charge to 3V, then to reaction pile constant-voltage charge 10 hours at 3V, after charging complete
Reaction pile is discharged to 0V；Slurry after aging is taken out from from reaction pile, with 2000 grams of benzene diluted slurries, is filtered,
Obtain pretreatment carbon nanotube；Pretreatment carbon nanotube is cleaned 3 times with 2600 grams of benzene, is dried at 200 DEG C.
With embodiment 1, test result is shown in Table 1 for electrode preparation, monomer assembling and test item.
Embodiment 6
1000 grams of activated carbon for super capacitors are weighed to be separately added into the positive pole zone and negative regions of reaction pile, it is close
Envelope reaction pile is evacuated to -0.098MPa for pile is reacted with vacuum pump；3400 grams are injected into reaction pile with topping-up pump
The SP2 type high-voltage electrolyte of SK group, South Korea, is stirred to react positive pole zone and the negative regions of pile with blender respectively, makes to surpass
Grade capacitor active carbon and the SP2 type high-voltage electrolyte of South Korea SK group form the slurry that solid content is 22.7wt%；It adjusts
The temperature of water bath with thermostatic control is to 60 DEG C, after reacting stack temperature and reaching stable, is connecting reaction pile just with charge-discharge test instrument
Pole collector and negative current collector first fill reaction pile constant-current charge to 2.85V, then at 2.85V to reaction pile constant pressure
Reaction pile is discharged to 0V after charging complete by electricity 10 hours；Slurry after aging is taken out from from reaction pile, with 2600
Gram ether diluted slurry, filtering obtain pretreatment activated carbon for super capacitors；Pretreatment activated carbon for super capacitors is used
3000 grams of ether clean 3 times, dry at 140 DEG C.
With embodiment 1, test result is shown in Table 1 for electrode preparation, monomer assembling and test item.
Comparative example 1
Commercial activated carbon for super capacitors is successively obtained after slurrying, coating, roll-in to the electrode with a thickness of 200 μm.
Electrode is cut into wide 35mm, positive length 570mm, cathode length 525mm.The super capacitor produced using Japanese NKK company
The dedicated TF4035 type diaphragm of device is wound into battery core together with the positive and negative anodes cut.60 battery cores are taken to be placed in 1M tetraethyl ammonium tetrafluoro
Vacuum impregnation is to saturation imbibition state in the solution in acetonitrile for boric acid, and by impregnated battery core loading shell, sealing obtains Φ
22*45 welding needle type supercapacitor monomer.Take 30 monomers at 60 DEG C with 2.7V constant pressure energization 1000 hours, observation monomer is
It is no that drum, the capacity of test unit and internal resistance has occurred.Remaining monomer is first with 5A constant-current charge to 2.7V, then with 5A constant-current discharge
It to 1.35V, and is recycled 100,000 times by this charge and discharge electric condition, whether observation monomer has occurred drum, the capacity and direct current of test unit
Internal resistance.Test result is shown in Table 1.
Comparative example 2
Commercial activated carbon for super capacitors is successively obtained after slurrying, coating, roll-in to the electrode with a thickness of 200 μm.
Electrode is cut into wide 35mm, positive length 570mm, cathode length 525mm.The super capacitor produced using Japanese NKK company
The dedicated TF4035 type diaphragm of device is wound into battery core together with the positive and negative anodes cut.60 battery cores are taken to be placed in 1M tetraethyl ammonium tetrafluoro
Boric acid vacuum impregnation extremely saturation imbibition state in the solution in acetonitrile, impregnated battery core is packed into shell, is equipped with interior survey
Lanthanum-nickel alloy cover board vacuum seal obtains Φ 22*45 welding needle type supercapacitor monomer.Take 30 monomers at 60 DEG C with
2.7V constant pressure is powered 1000 hours, and whether observation monomer has occurred drum, the capacity of test unit and internal resistance.Remaining monomer first with
5A constant-current charge is to 2.7V, then with 5A constant-current discharge to 1.35V, and recycles 100,000 times by this charge and discharge electric condition, observation monomer is
It is no that drum, the capacity and DC internal resistance of test unit has occurred.Test result is shown in Table 1.
Comparative example 3
Commercial activated carbon for super capacitors is successively obtained after slurrying, coating, roll-in to the electrode with a thickness of 200 μm.
Electrode is cut into wide 35mm, positive length 570mm, cathode length 525mm.The super capacitor produced using Japanese NKK company
The dedicated TF4035 type diaphragm of device is wound into battery core together with the positive and negative anodes cut.60 battery cores are taken to be placed in 1M tetraethyl ammonium tetrafluoro
Vacuum impregnation is to saturation imbibition state in the solution in acetonitrile for boric acid, to the battery core of the above-mentioned electrolyte of vacuum impregnation at 50 DEG C
With 2.7V constant pressure energization 10 hours, finally the battery core after energization aging is packed into shell, it is super to obtain Φ 22*45 welding needle type for sealing
Grade capacitor monomer.Take a part of gained monomer at 60 DEG C with 2.7V constant pressure energization 1000 hours, whether observation monomer is sent out
Drum, the capacity of test unit and internal resistance are given birth to.Remaining monomer is first with 5A constant-current charge to 2.7V, then extremely with 5A constant-current discharge
Whether 1.35V, and recycling 100,000 times by this charge and discharge electric condition, observation monomer have occurred drum, in the capacity and direct current of test unit
Resistance.Test result is shown in Table 1.
1 super capacitor electric core of table and monomer test result
According to the result of embodiment 1-6 it is found that with the pretreated supercapacitor electricity consumption of pretreatment unit of autonomous Design
The electrode of pole active material preparation, is assembled into Φ 22*45 welding needle type supercapacitor monomer, through high-temperature load 1000 hours or follows
Drum does not occur after ring 100,000 times, monomer capacity is 100F or more, and DC internal resistance is less than 12.5m Ω.Directly by super capacitor
Electrode assembling prepared by device active carbon is at Φ 22*45 welding needle type supercapacitor monomer, by 1 gained monomer of comparative example through high temperature
Load occurs obvious rise after 1000 hours or circulation 100,000 times and rouses, and capacity is lower than 90F, and DC internal resistance is greater than 22m Ω；By comparative example
2 gained monomers still occurred obvious rise through high-temperature load 1000 hours and rouse, and capacity attenuation and internal resistance increase effect are significant, monomer warp
Slight rise occurs after recycling 100,000 times to rouse, shows that lanthanum-nickel alloy in cover board has the part for absorbing and being generated by electrochemical action
The ability of mixed gas；Since the battery core of comparative example 3 has been undergone before being assembled into Φ 22*45 welding needle type supercapacitor monomer
Energization aging in 10 hours is roused although assembled monomer only occurs slightly to rise through high-temperature load 1000 hours or 10 Wan Cihou of circulation,
But monomer capacity is obviously relatively low, and DC internal resistance is also relatively large.
Claims (9)
1. a kind of electrode for super capacitor active material pretreatment unit, described device includes reaction pile, vacuum pump, charge and discharge
Electric tester, water bath with thermostatic control, topping-up pump and blender, which is characterized in that the outside for reacting pile is insulating layer, reacts pile
Inside is divided into positive pole zone and negative regions by intermediate diaphragm, and plus plate current-collecting body is located in the positive pole zone in reaction pile,
Negative current collector is located in the negative regions in reaction pile, and the positive pole zone and negative regions reacted in pile are respectively furnished with one
Blender reacts interface there are two the tops of pile, is connected respectively with topping-up pump and vacuum pump；The reaction pile anode collection
Body passes through insulating layer through lead-out wire and is connected with the positive terminal of charge-discharge test instrument, reacts pile negative current collector through lead-out wire
It is connected across insulating layer with the negative terminal of charge-discharge test instrument；The reaction pile is placed in water bath with thermostatic control.
2. electrode active material pretreatment unit according to claim 1, which is characterized in that the appearance of the reaction pile
Product is 10L, and top can freely open.
3. electrode active material pretreatment unit according to claim 1, which is characterized in that the plus plate current-collecting body or
The negative current collector is selected from aluminium, copper, silver, metal mesh or metal plate made of gold or platinum.
4. electrode active material pretreatment unit according to claim 1, which is characterized in that the diaphragm is selected from fiber
Plain diaphragm, polyethylene diagrams or polypropylene diaphragm.
5. a kind of preprocess method of electrode for super capacitor active material, which is characterized in that using as described in claim 1
Device, comprising the following steps:
1) electrode for super capacitor active material is separately added into the positive pole zone and negative regions of reaction pile, sealing is anti-
Pile is answered, is betted in vacuum degree≤- 0.098Mpa into super electrolyte for capacitor, coordination electrode active material and electrolyte shape
The slurry for being 10wt%-50wt% at range of solid content；
2) temperature of regulating thermostatic water-bath is to 60 DEG C -80 DEG C, with charge-discharge test instrument connect reaction pile plus plate current-collecting body and
Negative current collector, first by reaction pile constant-current charge to 2.5V-3.0V, then to reaction pile constant-voltage charge 8 at 2.5V-3.0V
Hour or more, pile will be reacted after charging complete is discharged to 0.1V hereinafter, completing the aging of slurry；
3) slurry after aging is taken out from reaction pile, with solvent reduction paste that is identical as electrolyte composition or can mixing
Material is washed out and obtained by drying to pretreatment electrode active material.
6. according to the method described in claim 5, it is characterized in that, the electrode active material be selected from active carbon, graphene,
Charcoal-aero gel or carbon nanotube.
7. according to the method described in claim 5, it is characterized in that, the supercapacitor is selected from tetraethyl ammonium with electrolyte
The second of the acetonitrile solution of tetrafluoro boric acid, the carbonic allyl ester solution of tetraethyl ammonium tetrafluoro boric acid, triethylmethylammonium tetrafluoro boric acid
The carbonic allyl ester solution of nitrile solution or triethylmethylammonium tetrafluoro boric acid.
8. the method according to the description of claim 7 is characterized in that the concentration of supercapacitor electrolyte is
0.7M-2.5M。
9. according to the method described in claim 5, it is characterized in that, the solvent be selected from acetonitrile, propene carbonate, chloroform,
One in carbon tetrachloride, benzene, normal propyl alcohol, isopropanol, acrylonitrile, ethyl acetate, dichloroethanes, ethyl alcohol, ether or carbon disulfide
Kind is a variety of.
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| CN101465417A (en) * | 2007-12-19 | 2009-06-24 | 中国科学院金属研究所 | Electrochemical treatment method for improving vanadium cell electrode material activity |
| CN104303357A (en) * | 2012-05-18 | 2015-01-21 | 丰田自动车株式会社 | Method for producing non-aqueous secondary battery |
| JP2014086382A (en) * | 2012-10-26 | 2014-05-12 | Kaneka Corp | Method for manufacturing nonaqueous electrolyte secondary battery, and battery manufactured by the method |
| CN104401992A (en) * | 2014-10-22 | 2015-03-11 | 深圳市贝特瑞新能源材料股份有限公司 | Method for preparing activated carbon for super capacitor with fruit shells as raw material and application of activated carbon |
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