CN106145110B - A kind of two step process for preparing activated of active carbon and its application in supercapacitor - Google Patents
A kind of two step process for preparing activated of active carbon and its application in supercapacitor Download PDFInfo
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Abstract
The invention discloses a kind of two step process for preparing activated of active carbon and its applications in supercapacitor, the described method comprises the following steps: by anthracite grinding and sieving, additive and binder stirring is added；It is put into Muffle furnace charing, is then transferred in tubular type activation furnace, activated gas activation is passed through；With dilute hydrochloric acid pickling, it is washed with distilled water after filtering, is impregnated with KOH solution；Activated carbon is put into activation furnace, protective gas activation is passed through；With dilute hydrochloric acid pickling, it is washed with distilled water to after filtering dry after pH is 7；Will be black and polytetrafluoroethylene (PTFE) uniformly mixes with ethylene after the grinding of re-activation deliming active carbon, it is coated in nickel foam, tabletting is prepared into capacitor after drying.For the present invention using anthracite as raw material, reaction condition is mild, on the basis of regular activated charcoal producing technique, by activating simultaneously deliming twice, greatly reduces synthesis cost, has huge popularization and application potentiality in high-performance super capacitor active carbon field.
Description
Technical field
The present invention relates to absorbent charcoal material preparation fields, and in particular to a kind of two step process for preparing activated of active carbon and its
Application in supercapacitor.
Background technique
Supercapacitor have high-energy density, high power density, have extended cycle life, stability is good, high/low temperature tolerance
It is strong and the advantages such as can be quickly charged and discharged, become the research hotspot of energy storage device.Active carbon is commonly electric as supercapacitor
Pole material, the reason is that active carbon stability is preferable, large specific surface area and price are suitable.The pore size of active carbon itself, hole
Shape and structure and the surface nature and supercapacitor chemical property of internal gutter between suffer from close connection, and
It is not that hole all in active carbon can form electric double layer, therefore, preparation is suitable as electrode material for super capacitor use
Active carbon first have to regulate and control the pore size of active carbon and distribution etc..
It is raw material that active carbon, which often uses coal, biomass (timber, coconut husk, stalk etc.), by carbonizing and activation is prepared.
Physically activated and chemical activation method is that active carbon prepares most common two methods.It is physically activated be with vapor, carbon dioxide,
Flue gas or air are the process that activator carries out high-temperature process；Chemical activation is to be with chemicals such as KOH, NaOH, ZnCl
Activator, the process activated at a proper temperature.Compared with physical activation method, the active carbon tool of chemical activation method preparation
There is richer microcellular structure.Suitable activation method and preparation process are the key that regulation activity charcoal holes.
With activated carbon pore size wider distribution prepared by physical activation method, regulate and control the active carbon based on middle micropore (< 10nm)
Difficulty is smaller (0-80F/g) as supercapacitor carbon material electrochemistry capacitance.Chemical activation method is often used activator and charcoal material
It is activated in a manner of physics blending, although can prepare, middle micropore is abundant, active carbon of large specific surface area, activator
Usage amount is big (activator and charcoal material mass ratio are generally higher than 1:1), expensive (90% about 8500 yuan of technical grade KOH price/
Ton), and activator utilization rate is lower, has very big corrosivity to equipment.Application No. is 201310536256.X, invention name
Referred to as disclosed in " method for preparation of active carbon " with raw material charcoal, KOH, assistant activator according to 1:1~7:0.001~0.1 weight
It than being activated at 600~850 DEG C after mixing, is then washed with water, salt acid elution, is washed with water and washs pH and reach 6~7, obtain
Activated carbon product specific surface area is greater than 2000m2/g.The patent prepares active carbon using physics blending KOH activation, and KOH makes
Dosage is 1 to 7 times of raw material charcoal.
Document " RSC Advances " " Facile synthesis of high-surface-area activated
carbon from coal for supercapacitors and high CO2It sorption. ", is 4:1 with KOH and coal dust
The blending of ratio physics carry out activation and prepare active carbon, active carbon specific surface area reaches 2457m2/ g, total pore volume 1.448mL/
G, microporosity 96.22%, using the speed of sweeping of 0.2V/s, to measure three-electrode system active carbon be the specific capacitance of electrode material for 279F/g.
Although the active carbon specific surface area of preparation, total pore volume and microporosity are higher, the specific capacitance for doing electrode material is also higher, KOH
Usage amount is 4 times of coal dust, and cost is very high, and KOH has extremely strong alkalinity and corrosivity, and a large amount of uses are to equipment corrosion
By force, the service life of equipment is greatly lowered.
Document " Acta PhySico-Chimica Sinica " " Effect of the activated carbon reactivation on its
Electrochemical capacitance. " carries out re-activation to active carbon at 850 DEG C using KOH as activator
And being washed to pH value is 7, the active carbon after re-activation is assembled into supercapacitor, measures electrochemistry capacitance and reaches 145.0F/
G, active carbon specific surface area are 1587m2/ g, aperture are concentrated mainly between 2-6nm, illustrate activated carbon pore size based on mesoporous,
But electrochemistry capacitance is not high.
The shortcomings that supercapacitor technologies prepared at present using active carbon from coal as electrode material includes: (1) general merchandise
The electrochemistry capacitance that active carbon prepares supercapacitor is generally lower；(2) the activated carbon capillary rate of physical activation method preparation is lower
And capacitance is low；(3) alkali activation method prepares that active carbon capacitance is big but at high cost, corrosive equipment.
Summary of the invention
The purpose of the present invention is to provide a kind of two step process for preparing activated of active carbon and its answering in supercapacitor
With by new method for preparation of active carbon, regulation activity charcoal distribution of pores prepares super capacitor under the premise of reducing cost
The high performance active carbon of device.
To achieve the above object, first aspect present invention provides a kind of two step process for preparing activated of active carbon.Specifically,
This method comprises the following steps:
Step 1: anthracite is smashed it through 200 meshes, 2~5% additive and the stirring of 3~8% binder is added
Mixture is made in 5~10min；
Step 2: the mixture glazing beads molding in step 1 is put into Muffle furnace with the heating rate liter of 5~15 DEG C/min
Temperature is cooled to room temperature to obtain carbonized material to 500~600 DEG C, and the tubular type that the carbonized material is then transferred to 700~900 DEG C is living
Change in furnace, is passed through activated gas and activates 1~2h, an activated carbon is made；
Step 3: concentration is 0.5~1mol/L under the conditions of 60~80 DEG C by an activated carbon in step 2
After dilute hydrochloric acid pickling 1~3 time, being washed with distilled water to pH value is 7, and then concentration is 5~15mol/L's under the conditions of 30 DEG C
KOH solution impregnates 1~12h；
Step 4: leading to being put into 500~900 DEG C of activation furnace in step 3 by an activated carbon of dipping
Enter protective gas and activate 0.5~3h, re-activation active carbon is made；
Step 5: concentration is 0.5~1mol/L under the conditions of 60~80 DEG C by the re-activation active carbon in step 4
After dilute hydrochloric acid pickling 1~3 time, being washed with distilled water to pH value is 7, obtains activated carbon for super capacitors material after dry；
Additive is one of potassium nitrate, sodium nitrate or magnesium nitrate in the step 1；Binder in the step 1
For one of coal tar, spent pulping liquor, molasses waste liquid or starch.
Preferably, anthracite is ash value less than 8% in the step 1.
Preferably, the activated gas in the step 2 is CO2Or vapor.
Preferably, the protective gas in the step 4 is N2。
Second aspect of the present invention provides a kind of application of activated carbon for super capacitors material, is used to prepare super capacitor
Device.
Preferably, will be black and polytetrafluoroethylene (PTFE) uniformly mixes with ethylene after active carbon grinding, coated in nickel foam,
Tabletting is prepared into capacitor after drying.
Preferably, the active carbon, ethylene carbon black and polytetrafluoroethylene (PTFE) are that 8:1:1 is uniformly mixed according to mass ratio.
Preferably, the electrolyte of the supercapacitor is the potassium hydroxide solution of 6mol/L.
The method of the present invention has the advantages that
1, the present invention is raw material using anthracite cheap and easy to get, is had the characteristics that inexpensive, easy to promote large-scale.
2, preparation method of the present invention is coupled in a manner of physically activated, chemical activation and three kinds of deliming, is carried out in preparation process
The activation of two steps, two step delimings, reaction system is simple, will not cause damages to environment.
3, chemical activation is deep into KOH in active carbon hole using the method for dipping KOH in preparation method of the present invention
Portion, is conducive to reaming, improves activation effect, and KOH dosage is greatly reduced, the burn into that reduces equipment reduces cost.
4, activated carbon for super capacitors material made from preparation method of the present invention, the uniform, microporosity with particle diameter distribution
The big feature of height, large specific surface area, total pore volume.
Detailed description of the invention
Fig. 1 is the process flow chart of the embodiment of the present invention 1.
Fig. 2 is cyclic voltammetry curve of the embodiment of the present invention 1 under 0.5A/g current density.
Fig. 3 is cyclic voltammetry curve of the embodiment of the present invention 2 under 0.5A/g current density.
Fig. 4 is cyclic voltammetry curve of the embodiment of the present invention 3 under 0.5A/g current density.
Fig. 5 is cyclic voltammetry curve of the embodiment of the present invention 4 under 0.5A/g current density.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
The preparation method of the present embodiment activated carbon for super capacitors material, sequentially includes the following steps:
One, the anthracite that ash value is 3.8% is smashed it through into 200 meshes, 4% potassium nitrate additive and 6% is added
Coal tar binder stir 5min, be made mixture；
Two, by the mixture glazing beads molding in step 1, Muffle furnace is put into the heating rate of 15 DEG C/min and is warming up to end
570 DEG C of temperature, cooling obtain carbonized material, are then transferred in 750 DEG C of tubular type activation furnace, are passed through steam activation 2h, are made one
Secondary activated carbon；
It three, with concentration is 0.6mol/L dilute hydrochloric acid pickling 3 under the conditions of 60 DEG C by an activated carbon in step 2
After secondary, being washed with distilled water to pH value is 7, then impregnates 6h with the KOH solution that concentration is 12mol/L under the conditions of 30 DEG C；
Four, it will be put into 500 DEG C of activation furnace by an activated carbon of dipping, be passed through N2Gas activates 1.2h, system
Obtain re-activation active carbon；
It five, with concentration is 0.5mol/L dilute hydrochloric acid pickling 3 under the conditions of 65 DEG C by the re-activation active carbon in step 4
After secondary, being washed with distilled water to pH value is 7, and activated carbon for super capacitors material (re-activation deliming activity is obtained after dry
Charcoal).
Embodiment 2
The preparation method of the present embodiment activated carbon for super capacitors material, sequentially includes the following steps:
One, it is that 6% anthracite smashes it through 200 meshes by ash value, 5% potassium nitrate additive and 8% coal is added
Tar binder stirs 6min, and mixture is made；
Two, by the mixture glazing beads molding in step 1, Muffle furnace is put into the heating rate of 5 DEG C/min and is warming up to final temperature
600 DEG C, cooling obtains carbonized material, is then transferred in 700 DEG C of tubular type activation furnace, is passed through CO2Gas activation 1.5h is made one
Secondary activated carbon；
It three, with concentration is 0.5mol/L dilute hydrochloric acid pickling 1 under the conditions of 70 DEG C by an activated carbon in step 2
After secondary, being washed with distilled water to pH value is 7, then impregnates 10h with the KOH solution that concentration is 8mol/L under the conditions of 30 DEG C；
Four, it will be put into 800 DEG C of activation furnace by an activated carbon of dipping, be passed through N2Gas activates 1h, is made
Re-activation active carbon；
It five, with concentration is 0.9mol/L dilute hydrochloric acid pickling 2 under the conditions of 80 DEG C by the re-activation active carbon in step 4
After secondary, being washed with distilled water to pH value is 7, and activated carbon for super capacitors material (re-activation deliming activity is obtained after dry
Charcoal).
Embodiment 3
The preparation method of the present embodiment activated carbon for super capacitors material, sequentially includes the following steps:
One, it is that 8% anthracite smashes it through 200 meshes by ash value, 2% potassium nitrate additive and 5% coal is added
Tar binder stirs 10min, and mixture is made；
Two, by the mixture glazing beads molding in step 1, Muffle furnace is put into the heating rate of 8 DEG C/min and is warming up to final temperature
560 DEG C, cooling obtains carbonized material, is then transferred in 850 DEG C of tubular type activation furnace, is passed through vapor body activation 1.3h, is made
Activated carbon；
It three, with concentration is 1mol/L dilute hydrochloric acid pickling 2 times under the conditions of 75 DEG C by an activated carbon in step 2
Afterwards, being washed with distilled water to pH value is 7, then impregnates 1h with the KOH solution that concentration is 15mol/L under the conditions of 30 DEG C；
Four, it will be put into 700 DEG C of activation furnace by an activated carbon of dipping, be passed through N2Gas activates 3h, is made
Re-activation active carbon；
It five, with concentration is 0.7mol/L dilute hydrochloric acid pickling 1 under the conditions of 75 DEG C by the re-activation active carbon in step 4
After secondary, being washed with distilled water to pH value is 7, and activated carbon for super capacitors material (re-activation deliming activity is obtained after dry
Charcoal).
Embodiment 4
The preparation method of the present embodiment activated carbon for super capacitors material, sequentially includes the following steps:
One, it is that 4% anthracite smashes it through 200 meshes by ash value, 3% potassium nitrate additive and 3% coal is added
Tar binder stirs 8min, and mixture is made；
Two, by the mixture glazing beads molding in step 1, Muffle furnace is put into the heating rate of 12 DEG C/min and is warming up to end
540 DEG C of temperature, cooling obtain carbonized material, are then transferred in 900 DEG C of tubular type activation furnace, are passed through CO2Gas activation 1h is made one
Secondary activated carbon；
It three, with concentration is 0.8mol/L dilute hydrochloric acid pickling 2 under the conditions of 80 DEG C by an activated carbon in step 2
After secondary, being washed with distilled water to pH value is 7, then impregnates 12h with the KOH solution that concentration is 5mol/L under the conditions of 30 DEG C；
Four, it will be put into 900 DEG C of activation furnace by an activated carbon of dipping, be passed through N2Gas activates 0.5h, system
Obtain re-activation active carbon；
It five, with concentration is 1mol/L dilute hydrochloric acid pickling 1 time under the conditions of 60 DEG C by the re-activation active carbon in step 4
Afterwards, being washed with distilled water to pH value is 7, and activated carbon for super capacitors material (re-activation deliming activity is obtained after dry
Charcoal).
Embodiment 5
The preparation method of the present embodiment supercapacitor, sequentially includes the following steps:
Will by Examples 1 to 4 method prepare activated carbon for super capacitors material grinding after with ethylene carbon black and gather
Tetrafluoroethene is uniformly mixed according to 8:1:1, is coated in nickel foam, and tabletting is prepared into capacitor after drying, wherein capacitor
Electrolyte is the potassium hydroxide solution of 6mol/L.
The average pore size of the activated carbon for super capacitors material that 1 Examples 1 to 4 of table is prepared, total pore volume and compare table
Area
From table 1 it follows that the average pore size of activated carbon for super capacitors material made from Examples 1 to 4 exists
1.7nm left and right；Microporosity is 89% or more, and total pore volume is in 0.4mL/g or so；Specific surface area is in 860cm2/ g or more,
The capacitor absorbent charcoal material produced much higher than existing preparation method.
The activated carbon for super capacitors material that 2 Examples 1 to 4 of table is prepared is respectively according to the super electricity of embodiment 5
The performance indicator for the supercapacitor that the preparation method of container is prepared
From Table 2, it can be seen that the activated carbon for super capacitors material being prepared with Examples 1 to 4 is according to implementation
The supercapacitor that the preparation method of the supercapacitor of example 5~8 is prepared, under 0.5A/g current density, active carbon ratio
Capacitor after 240F/g or more, cycle charge-discharge 5000 times specific capacitance sustainment rate 99% or more.In addition, such as the institute of Fig. 2~5
Show, the activated carbon for super capacitors material being prepared with the preparation method of Examples 1 to 4 is respectively according to the super of embodiment 5
The supercapacitor of the preparation method preparation of grade capacitor, has typical electric double layer capacitance type cyclic voltammetry curve, performance
Remote super existing product.
A kind of the advantages of two step process for preparing activated of activated carbon for super capacitors material of the present invention, is, uses we
The electrochemistry index of the active carbon of method preparation reaches advanced international level, compared with other electrode material for super capacitor of same level
Cost is greatly lowered.There is certain pore structure, first time pore-creating by physically activated obtain a activated carbon；
The remaining ash content of pore interior, second of help reaming are removed by pickling water elution；Primary activation deliming active carbon is molten by KOH
Liquid impregnation, KOH are adsorbed in active carbon hole, and KOH can activate pore-creating in pore interior when re-activation, and third time is helped
Help pore-creating and reaming；Pickling water elution is except the ash contents such as the minerals of active carbon pore interior, the 4th help reaming again.It is this
The method of multiple pore-creating and reaming can prepare the active carbon of pore structure prosperity.
Physics blends the method that KOH carries out chemical activation, although the activity of bigger serface, macroporosity can be prepared
Charcoal, but because being surface contact between KOH and coal dust, it can not be deep into inside coal dust and carry out pore-creating.It is primary to activate in this method
Active carbon afterwards has had more developed pore structure, and subsequent progress KOH impregnation reactivation blends KOH method with physics
The process for preparing active carbon compares, and KOH can be adsorbed onto active carbon hole depths in this method, in re-activation,
KOH can carry out in turn pore-creating and reaming with the charcoal substrate reaction of pore interior, more targeted for the exploitation of deep hole,
It is more conducive to the reaming of micropore.In addition, physics blending activation method is usually using KOH (the general KOH mass for being multiple times than quality of pc
It is 2~8 times of quality of pc), KOH usage amount is only the 10% of quality of pc when KOH infusion process prepares re-activation active carbon
~60%, it reduces costs.Secondly, physics blending activation method is put into activation furnace progress after directly mixing KOH powder with coal dust
Activation, KOH are directly contacted with activation furnace inner wall, because KOH has strong basicity and strong corrosive, easily corrode activation furnace inner wall, if
Standby service life is short；For this method using being activated after dipping KOH, KOH has been deep into active carbon pore interior, activation process
Middle KOH directly with the charcoal substrate reaction pore-creating of active carbon, will not directly be contacted with activation furnace, so corrosivity substantially reduces, it can
Extend the service life of activation furnace.
Although above having used general explanation and specific embodiment, the present invention is described in detail, at this
On the basis of invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore,
These modifications or improvements without departing from theon the basis of the spirit of the present invention are fallen within the scope of the claimed invention.
Claims (7)
1. a kind of two step process for preparing activated of activated carbon for super capacitors, which is characterized in that the method includes following step
It is rapid:
Step 1: anthracite is smashed it through 200 meshes, be added 2~5% additive and 3~8% binder stirring 5~
Mixture is made in 10min；
Step 2: the mixture glazing beads molding in step 1 to be put into Muffle furnace and is warming up to the heating rate of 5~15 DEG C/min
It 500~600 DEG C, is cooled to room temperature to obtain carbonized material, then the carbonized material is transferred to 700~900 DEG C of tubular type activation furnace
In, it is passed through activated gas and activates 1~2h, an activated carbon is made；
Step 3: concentration is the dilute salt of 0.5~1mol/L under the conditions of 60~80 DEG C by an activated carbon in step 2
After pickling 1~3 time, being washed with distilled water to pH value is 7, the KOH that then concentration is 5~15mol/L under the conditions of 30 DEG C
Solution impregnates 1~12h；
Step 4: being passed through guarantor for being put into 500~900 DEG C of activation furnace in step 3 by an activated carbon of dipping
0.5~3h of gas activation is protected, re-activation active carbon is made；
Step 5: concentration is the dilute salt of 0.5~1mol/L under the conditions of 60~80 DEG C by the re-activation active carbon in step 4
After pickling 1~3 time, being washed with distilled water to pH value is 7, obtains activated carbon for super capacitors material after dry；
Additive is one of potassium nitrate, sodium nitrate or magnesium nitrate in the step 1；Binder is coal in the step 1
One of tar, spent pulping liquor, molasses waste liquid or starch.
2. two step process for preparing activated of activated carbon for super capacitors according to claim 1, it is characterised in that: the step
Anthracite ash value is less than 8% in rapid one.
3. two step process for preparing activated of activated carbon for super capacitors according to claim 1, it is characterised in that: the step
Activated gas in rapid two is CO2Or vapor.
4. two step process for preparing activated of activated carbon for super capacitors according to claim 1, it is characterised in that: the step
Protective gas in rapid four is N2。
5. active carbon made from the described in any item two step process for preparing activated of activated carbon for super capacitors of claim 1-4
Using, it is characterised in that: the active carbon is used to prepare supercapacitor.
6. the application of activated carbon for super capacitors according to claim 5, it is characterised in that: the supercapacitor
Preparation method is coated in and steeps the following steps are included: by black and polytetrafluoroethylene (PTFE) uniformly mixes with ethylene after active carbon grinding
On foam nickel, tabletting is prepared into capacitor after drying.
7. the application of activated carbon for super capacitors according to claim 6, it is characterised in that: the active carbon, ethylene
Carbon black and polytetrafluoroethylene (PTFE) are uniformly mixed according to mass ratio for 8:1:1.
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| CN102205962B (en) * | 2011-03-10 | 2013-03-06 | 安徽工业大学 | Device and method for preparing activated carbon material for electrochemical capacitor |
| CN102442664A (en) * | 2011-09-29 | 2012-05-09 | 朱海生 | Production method for bamboo electric double layer capacitor electrode active carbon |
| CN102701201B (en) * | 2012-06-21 | 2015-11-18 | 山东大学 | A kind of lignin from alkaline paper-making black liquor prepares the method for Powdered Activated Carbon |
| CN104649265A (en) * | 2015-02-04 | 2015-05-27 | 昆明理工大学 | Method for preparing active carbon with high specific surface area from walnut shell |
| CN105060290B (en) * | 2015-07-16 | 2017-03-01 | 陕西煤业化工技术研究院有限责任公司 | A kind of preparation method of ature of coal low ash high specific surface area active carbon |
| CN105384169B (en) * | 2015-12-09 | 2017-10-24 | 湖北汽车工业学院 | A kind of preparation method of electrode of super capacitor activated carbon |
| CN105502379A (en) * | 2015-12-31 | 2016-04-20 | 中国矿业大学 | Preparation method of active carbon for adsorbing and separating carbon dioxide |
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2016
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