CN105869920B - A kind of preparation method of ultracapacitor carbon material - Google Patents
A kind of preparation method of ultracapacitor carbon material Download PDFInfo
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- CN105869920B CN105869920B CN201610193225.2A CN201610193225A CN105869920B CN 105869920 B CN105869920 B CN 105869920B CN 201610193225 A CN201610193225 A CN 201610193225A CN 105869920 B CN105869920 B CN 105869920B
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Abstract
The preparation method of ultracapacitor carbon material disclosed in this invention, comprises the following steps：Manioc waste is put into water, adds pre- preserved material, is presoaked 30 minutes；Then charging heat temperature raising, maintains 80~90 minutes when pressure rises to 0.8~1MPa, opens explosion；Wash with water, extruding drying, under nitrogen protection, is warming up to 1000 DEG C, when constant temperature 2 is small, obtains carbon material；Obtained carbon material is mixed with graphite, beta cyclodextrin, this mixture is modulated into half siccative with alcohol, grinding is uniform and is pressed into piece, is washed into disk, is pressed into two panels nickel foam, when 100~110 DEG C of vacuum drying 20~24 are small, obtained battery pole piece.
Description
Technical field
The invention belongs to capacitor technology field, and in particular to a kind of preparation method of ultracapacitor carbon material.
Background technology
Ultracapacitor is called double layer capacitor, is a kind of electrochemical element, but does not occur in the process of its energy storage
Chemical reaction, and the Electro Sorb and desorption process of anions and canons simply occur on two porous positive and negative pole plate, it is this
Thermal energy storage process completely reversibility, also just because of this ultracapacitor can be hundreds thousand of times with repeated charge.Ultracapacitor can be with
It is considered as the two reactionless active porous electrode plates to suspend in the electrolyte, is powered up on pole plate, positive plate attracts electrolysis
Anion in matter, negative plate attract cation, actually form two capacitive accumulation layers, the cation being separated is in anode
Near plate, anion is near positive plate.
It is as follows as the ultracapacitor principle of active material using porous carbon：When applied voltage is added to two of ultracapacitor
When on pole plate, as ordinary capacitor, the positive electrode storage positive charge of pole plate, negative plate storage negative electrical charge, in super capacitor
Under the electric field action that electric charge produces on the two-plate of device, in electrolyte with forming opposite electric charge on interelectrode interface, with flat
Weigh the internal electric field of electrolyte, and this positive charge and negative electrical charge are on the contact surface between two different phases, between positive and negative charge
For extremely short gap arrangement on opposite position, this charge distribution layers is called electric double layer.Since capacitance and polar board surface product are into just
Than, and the spacing between positive and negative charge is inversely proportional, and the specific surface area that the polar plate area of ultracapacitor is porous carbon, generally
For 1000~3000m2/ g, the surface area than traditional capacitor are more than 3~4 orders of magnitude, in ultracapacitor positive and negative charge it
Between be spaced about 0.5nm, therefore the capacity of ultracapacitor is very big, can reach 1~5000F, the electricity of part special designing
Container is even up to surprising 100,000 farads.
The critical material for determining performance of the supercapacitor quality is its electrode material, and the electrode material of ultracapacitor is mostly
Using porous carbon materials, generally require specific surface area the higher the better, for same type of material, specific surface area is bigger, material
Electric conductivity it is lower, while pore volume is bigger.But the exigent power density of ultracapacitor and certain volume energy storage density,
Therefore there is certain requirement to the electric conductivity and pore volume of material, electric conductivity is the higher the better, and pore volume is about 1.0~1.3cm3/
g.In the prior art, porous carbon materials good conductivity, it is of high cost；Cost is low, and electric conductivity is poor.
The Chinese invention patent (publication date for 2010 on August 11) of Publication No. CN101800131A discloses a kind of work
Property carbon-based material and preparation method thereof, using under inert gas shielding, doped or undoped polyaniline polymer is existed
500-1200 DEG C of carbonization 1-24h, then carries out high-temperature activation or solution activation process, and the high-temperature activation is by after carbonization
Material and activator keep the temperature 0-20h at 100-1000 DEG C, the solution activation be by the material after carbonization sulfuric acid, nitric acid,
0.5-96h is soaked in the solution of hydrochloric acid, potassium permanganate, hydrogen peroxide etc..But the specific surface area of carbon material made from this method
Still it is smaller, limit further improving for its specific capacitance.
The content of the invention
Goal of the invention：For shortcoming of the prior art, the present invention provides a kind of ultracapacitor carbon material
Preparation method.
Technical solution：The preparation method of ultracapacitor carbon material provided by the present invention, comprises the following steps：
Manioc waste is put into water, adds pre- preserved material, is presoaked 30~40 minutes；Then charging heat temperature raising, when in pressure
Maintained 80~90 minutes when being raised to 0.8~1.2MPa, open explosion；Wash with water, extruding drying, under nitrogen protection, is warming up to
1000~1200 DEG C, when constant temperature 2~3 is small, obtain carbon material；
Obtained carbon material is mixed with graphite, beta-cyclodextrin, this mixture is modulated into half siccative with alcohol, is ground
Uniformly and piece is pressed into, is washed into disk, be pressed into two panels nickel foam, when 100~110 DEG C of vacuum drying 20~24 are small, battery is made
Use pole piece.
The pre- preserved material is NaOH and Na2SO3Mixture, both mass ratioes be 4:1.The pre- preserved material quality
Concentration is 3%.
The heating rate is 10 DEG C/min.
The mass ratio of the carbon material and graphite, beta-cyclodextrin is 80:10:10.
For the battery pole piece using platinized platinum as to electrode, electrolyte is 6mol/L potassium hydroxide solutions, is lied prostrate using circulation
The specific capacitance of peace method test material.
Further, preferred solution of the invention is：
Weigh 100g manioc wastes to put into the bucket equipped with 3L water, add pre- preserved material (NaOH：Na2SO3=4:1), pre- preserved material
Concentration is 3%, is presoaked 30 minutes；Then charging heat temperature raising, maintains 80 minutes when pressure rises to 0.8MPa, opens explosion；
Wash with water, extruding drying, under nitrogen protection, with speed, be warming up to 1000 DEG C, when constant temperature 2 is small, obtain carbon material；
By obtained carbon material and graphite, binding agent beta-cyclodextrin according to mass ratio 80:10:10 mixing, will with alcohol
This mixture is modulated into half siccative, and grinding is uniform and is pressed into piece, is washed into disk, is pressed into two panels nickel foam, 100 DEG C of vacuum drying
24 it is small when, obtained experimental cell pole piece.Using platinized platinum as to electrode, electrolyte is 6mol/L potassium hydroxide solutions, using circulation
The specific capacitance of voltammetry test material.
Beneficial effect：The ultracapacitor of the present invention is simple with the preparation method of nitrogenous carbon material, and the cost of raw material is cheap,
Easily realize large-scale production.The ultracapacitor prepared using obtained ultracapacitor with nitrogenous carbon material has higher ratio
Capacity.
Embodiment：
Embodiment 1
Weigh 100g manioc wastes to put into the bucket equipped with 3L water, add pre- preserved material (NaOH：Na2SO3=4:1), pre- preserved material
Concentration is 3%, is presoaked 30 minutes；Then charging heat temperature raising, maintains 80 minutes when pressure rises to 0.8MPa, opens explosion；
Wash with water, extruding drying, under nitrogen protection, with 10 DEG C/min of speed, is warming up to 1000 DEG C, when constant temperature 2 is small, obtains
Carbon material.
By obtained carbon material and graphite, beta-cyclodextrin according to mass ratio 80:10:10 mixing, are mixed this with alcohol
Thing is modulated into half siccative, and grinding is uniform and is pressed into piece, is washed into disk, is pressed into two panels nickel foam, and 100 DEG C of vacuum drying 24 are small
When, obtained experimental cell pole piece.Using platinized platinum as to electrode, electrolyte is 6mol/L potassium hydroxide solutions, using cyclic voltammetric
The specific capacitance of method test material.
Material as made by the present embodiment, during with the velocity scanning of 10mV/s, specific capacitance 325F/g.
Embodiment 2
Weigh 100g manioc wastes to put into the bucket equipped with 3L water, add pre- preserved material (NaOH：Na2SO3=4:1), pre- preserved material
Concentration is 3%, is presoaked 40 minutes；Then charging heat temperature raising, maintains 80 minutes when pressure rises to 1MPa, opens explosion；With
Water cleans, and extruding drying, under nitrogen protection, with 10 DEG C/min of speed, is warming up to 1000 DEG C, when constant temperature 2 is small, obtains carbon
Material.
By obtained carbon material and graphite, beta-cyclodextrin according to mass ratio 80:10:10 mixing, are mixed this with alcohol
Thing is modulated into half siccative, and grinding is uniform and is pressed into piece, is washed into disk, is pressed into two panels nickel foam, and 100 DEG C of vacuum drying 20 are small
When, obtained experimental cell pole piece.Using platinized platinum as to electrode, electrolyte is 6mol/L potassium hydroxide solutions, using cyclic voltammetric
The specific capacitance of method test material.
Material as made by the present embodiment, during with the velocity scanning of 10mV/s, specific capacitance 335F/g.
Embodiment 3
Weigh 100g manioc wastes to put into the bucket equipped with 3L water, add pre- preserved material (NaOH：Na2SO3=4:1), pre- preserved material
Concentration is 3%, is presoaked 40 minutes；Then charging heat temperature raising, maintains 80 minutes when pressure rises to 1.2MPa, opens explosion；
Wash with water, extruding drying, under nitrogen protection, with 10 DEG C/min of speed, is warming up to 1000 DEG C, when constant temperature 2 is small, obtains
Carbon material.
By obtained carbon material and graphite, beta-cyclodextrin according to mass ratio 80:10:10 mixing, are mixed this with alcohol
Thing is modulated into half siccative, and grinding is uniform and is pressed into piece, is washed into disk, is pressed into two panels nickel foam, and 110 DEG C of vacuum drying 20 are small
When, obtained experimental cell pole piece.Using platinized platinum as to electrode, electrolyte is 6mol/L potassium hydroxide solutions, using cyclic voltammetric
The specific capacitance of method test material.
Material as made by the present embodiment, during with the velocity scanning of 10mV/s, specific capacitance 333F/g.
Embodiment 4
Weigh 200g manioc wastes to put into the bucket equipped with 3L water, add pre- preserved material (NaOH：Na2SO3=4:1), pre- preserved material
Concentration is 3%, is presoaked 40 minutes；Then charging heat temperature raising, maintains 90 minutes when pressure rises to 1MPa, opens explosion；With
Water cleans, and extruding drying, under nitrogen protection, with 10 DEG C/min of speed, is warming up to 1200 DEG C, when constant temperature 2 is small, obtains carbon
Material.
By obtained carbon material and graphite, beta-cyclodextrin according to mass ratio 80:10:10 mixing, are mixed this with alcohol
Thing is modulated into half siccative, and grinding is uniform and is pressed into piece, is washed into disk, is pressed into two panels nickel foam, and 110 DEG C of vacuum drying 20 are small
When, obtained experimental cell pole piece.Using platinized platinum as to electrode, electrolyte is 6mol/L potassium hydroxide solutions, using cyclic voltammetric
The specific capacitance of method test material.
Material as made by the present embodiment, during with the velocity scanning of 10mV/s, specific capacitance 341F/g.
Embodiment 5
Weigh 150g manioc wastes to put into the bucket equipped with 3L water, add pre- preserved material (NaOH：Na2SO3=4:1), pre- preserved material
Concentration is 3%, is presoaked 40 minutes；Then charging heat temperature raising, maintains 90 minutes when pressure rises to 1MPa, opens explosion；With
Water cleans, and extruding drying, under nitrogen protection, with 10 DEG C/min of speed, is warming up to 1100 DEG C, when constant temperature 3 is small, obtains carbon
Material.
By obtained carbon material and graphite, beta-cyclodextrin according to mass ratio 80:10:10 mixing, are mixed this with alcohol
Thing is modulated into half siccative, and grinding is uniform and is pressed into piece, is washed into disk, is pressed into two panels nickel foam, and 110 DEG C of vacuum drying 22 are small
When, obtained experimental cell pole piece.Using platinized platinum as to electrode, electrolyte is 6mol/L potassium hydroxide solutions, using cyclic voltammetric
The specific capacitance of method test material.
Material as made by the present embodiment, during with the velocity scanning of 10mV/s, specific capacitance 343F/g.
Embodiment 6
Weigh 120g manioc wastes to put into the bucket equipped with 3L water, add pre- preserved material (NaOH：Na2SO3=4:1), pre- preserved material
Concentration is 3%, is presoaked 45 minutes；Then charging heat temperature raising, maintains 80 minutes when pressure rises to 1.2MPa, opens explosion；
Wash with water, extruding drying, under nitrogen protection, with 10 DEG C/min of speed, is warming up to 1100 DEG C, when constant temperature 3 is small, obtains
Carbon material.
By obtained carbon material and graphite, beta-cyclodextrin according to mass ratio 80:10:10 mixing, are mixed this with alcohol
Thing is modulated into half siccative, and grinding is uniform and is pressed into piece, is washed into disk, is pressed into two panels nickel foam, and 110 DEG C of vacuum drying 22 are small
When, obtained experimental cell pole piece.Using platinized platinum as to electrode, electrolyte is 6mol/L potassium hydroxide solutions, using cyclic voltammetric
The specific capacitance of method test material.
Material as made by the present embodiment, during with the velocity scanning of 10mV/s, specific capacitance 339F/g.
Claims (5)
1. a kind of preparation method of ultracapacitor carbon material, it is characterised in that comprise the following steps：
Manioc waste is put into water, adds pre- preserved material, is presoaked 30 ~ 40 minutes；Then charging heat temperature raising, when pressure rises to
Maintained 80 ~ 90 minutes during 0.8 ~ 1.2MPa, open explosion；Wash with water, extruding drying, under nitrogen protection, it is warming up to 1000 ~
1200 DEG C, when constant temperature 2 ~ 3 is small, obtain carbon material；
Obtained carbon material is mixed with graphite, beta-cyclodextrin, this mixture is modulated into half siccative with alcohol, grinding is uniform
And piece is pressed into, and disk is washed into, is pressed into two panels nickel foam, when 100 ~ 110 DEG C of vacuum drying 20 ~ 24 are small, obtained battery pole piece；
The pre- preserved material is NaOH and Na2SO3Mixture, both mass ratioes be 4:1；
The pre- preserved material mass concentration is 3%.
2. the preparation method of ultracapacitor carbon material according to claim 1, it is characterised in that the speed of the heating
Rate is 10 DEG C/min.
3. the preparation method of ultracapacitor carbon material according to claim 1, it is characterised in that the carbon material with
Graphite, the mass ratio of beta-cyclodextrin are 80: 10 : 10.
4. the preparation method of ultracapacitor carbon material according to claim 1, it is characterised in that the battery pole
Piece is using platinized platinum as to electrode, and electrolyte is 6mol/L potassium hydroxide solutions, using the specific capacitance of cyclic voltammetry test material.
5. the preparation method of ultracapacitor carbon material according to claim 1, it is characterised in that：
Weigh 100g manioc wastes to put into the bucket equipped with 3L water, add pre- preserved material, the pre- preserved material is NaOH and Na2SO3It is mixed
And thing, NaOH and Na2SO3Mass ratio be 4:1, preimpregnation agent concentration is 3%, is presoaked 30 minutes；Then charging heat temperature raising, works as pressure
Power maintains 80 minutes when rising to 0.8MPa, opens explosion；Wash with water, extruding drying, under nitrogen protection, with 10 DEG C/min
Speed, be warming up to 1000 DEG C, when constant temperature 2 is small, obtain carbon material；By obtained carbon material and graphite, beta-cyclodextrin according to
Mass ratio 80: 10 :10 mixing, are modulated into half siccative, grinding is uniform and is pressed into piece, is washed into circle with alcohol by this mixture
Piece, is pressed into two panels nickel foam, and when 100 DEG C of vacuum drying 24 are small, experimental cell pole piece is made, using platinized platinum as to electrode, electricity
Solution liquid is 6mol/L potassium hydroxide solutions, using the specific capacitance of cyclic voltammetry test material.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101697322A (en) * | 2009-10-15 | 2010-04-21 | 青岛大学 | Method for preparing porous carbon electrode material |
| CN102280262A (en) * | 2011-01-24 | 2011-12-14 | 青岛大学 | Porous carbon electrode material and preparing method thereof |
| CN103183329A (en) * | 2013-03-19 | 2013-07-03 | 燕山大学 | Preparation method of multistage-channel carbon electrode material |
| CN104766726A (en) * | 2015-04-29 | 2015-07-08 | 上海博暄能源科技有限公司 | Preparation method for supercapacitor electrode material and electrode material prepared through same |
| CN105244178A (en) * | 2015-10-28 | 2016-01-13 | 王彦博 | Super capacitor and preparation method thereof |
-
2016
- 2016-03-30 CN CN201610193225.2A patent/CN105869920B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101697322A (en) * | 2009-10-15 | 2010-04-21 | 青岛大学 | Method for preparing porous carbon electrode material |
| CN102280262A (en) * | 2011-01-24 | 2011-12-14 | 青岛大学 | Porous carbon electrode material and preparing method thereof |
| CN103183329A (en) * | 2013-03-19 | 2013-07-03 | 燕山大学 | Preparation method of multistage-channel carbon electrode material |
| CN104766726A (en) * | 2015-04-29 | 2015-07-08 | 上海博暄能源科技有限公司 | Preparation method for supercapacitor electrode material and electrode material prepared through same |
| CN105244178A (en) * | 2015-10-28 | 2016-01-13 | 王彦博 | Super capacitor and preparation method thereof |
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Inventor after: Yan Xueqing Inventor after: Wang Shuangyin Inventor after: Zhao Rongxing Inventor after: Deng Shuguang Inventor after: Li Zhe Inventor after: Jiang Wei Inventor after: Chen Zhiyong Inventor after: Qian Jun Inventor after: Tang Lei Inventor before: Wang Shuangyin Inventor before: Yan Xueqing Inventor before: Xu Wenyong Inventor before: Zhao Rongxing Inventor before: Tan Naiyun |
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Effective date of registration: 20180404 Address after: 88 No. 225600 Jiangsu city of Yangzhou province Gaoyou Bosideng Road Economic Development Zone Applicant after: Jiangsu Oliter Energy Technology Co., Ltd. Address before: 225600 Gaoyou City, Jiangsu Province Economic Development Zone, Dongting Lake Road, science and technology center, Applicant before: Yangzhou Kaben Carbon Energy Technology Co., Ltd. |
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