CN107879343A - A kind of preparation method of super capacitor carbon - Google Patents
A kind of preparation method of super capacitor carbon Download PDFInfo
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- CN107879343A CN107879343A CN201711114036.2A CN201711114036A CN107879343A CN 107879343 A CN107879343 A CN 107879343A CN 201711114036 A CN201711114036 A CN 201711114036A CN 107879343 A CN107879343 A CN 107879343A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000003990 capacitor Substances 0.000 title claims abstract description 57
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 40
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 40
- 235000005822 corn Nutrition 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 12
- 238000003763 carbonization Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 7
- 238000005238 degreasing Methods 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims abstract description 3
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 50
- 240000008042 Zea mays Species 0.000 claims description 38
- 229910052757 nitrogen Inorganic materials 0.000 claims description 25
- 239000000463 material Substances 0.000 claims description 23
- 238000001994 activation Methods 0.000 claims description 22
- 230000004913 activation Effects 0.000 claims description 21
- 238000000354 decomposition reaction Methods 0.000 claims description 12
- 239000008188 pellet Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 7
- 238000000197 pyrolysis Methods 0.000 claims description 7
- 238000003801 milling Methods 0.000 claims description 6
- 238000009700 powder processing Methods 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000037452 priming Effects 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 235000013312 flour Nutrition 0.000 claims description 4
- 229920002521 macromolecule Polymers 0.000 claims description 4
- 239000005416 organic matter Substances 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000003518 caustics Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims description 2
- 238000007865 diluting Methods 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 241000209149 Zea Species 0.000 abstract 2
- 238000002203 pretreatment Methods 0.000 abstract 1
- 241000209094 Oryza Species 0.000 description 6
- 235000007164 Oryza sativa Nutrition 0.000 description 6
- 235000009566 rice Nutrition 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 4
- 239000010977 jade Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000035568 catharsis Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of super capacitor carbon, using corn as raw material, carries out the pre-treatment of corn degreasing deliming first, then temperature-gradient method removes moisture removal and low temperature volatile matter, is prepared into carbonization presoma.Physical and chemical method is respectively adopted respectively to activate presoma progress high-temperature vapor and highly basic, obtain the porous activated carbon of different index performances, free from admixture Oxidation Doping and forming processes are finally carried out respectively, the super capacitor carbon of different index performances is obtained, using ratio surface >=1800m of super capacitor carbon made from Physical2/g;Specific capacity >=160F/g, tap density >=0.30g/cm3, the Ω m of resistivity≤2.0, particle diameter distribution D50≤17 μm, ash content≤0.2%;Using ratio surface >=1700m of super capacitor carbon made from chemical method2/g;Specific capacity >=260F/g, tap density >=0.30g/cm3, the Ω m of resistivity≤2.0, particle diameter distribution D50≤17 μm, ash content≤0.2%.
Description
Technical field
The present invention relates to electrochemical capacitor field, particularly a kind of preparation method of super capacitor carbon.
Background technology
Ultracapacitor is also referred to as electrochemical capacitor, generally its specific capacitance is big, good cycling stability, work
The features such as principle is simple, power density is high, charge/discharge rates are fast and turn into focus of concern gradually, meanwhile, it is also with two
Primary cell combination can realize the complementation than energy and specific power and be applied to the fields such as electric car power supply and power engineering.
Mainly there are three classes, respectively carbon materials, metal oxygen currently used for the material used in ultracapacitor polarizing electrode
Compound material and conducting polymer materials.Common carbon materials is activated carbon, because it has high-specific surface area, electrochemistry
Can be very remarkable excellent, turn into a kind of electrode material of scientists extensive concern gradually.But in general activated carbon electrodes
Material source is in ature of coal and wooden raw material, and ash content is high, and electric conductivity is low, and cyclicity is poor, than electricity under the conditions of high power charging-discharging
It is fast to hold decay, it is difficult to meet the use demand of ultracapacitor.Other materials such as graphene, CNT etc. are by cost and technology
Restriction, commercialization progress is slower, and really practical low cost, Large Copacity, fast charging and discharging problem are still unresolved.Cause
This, it would be highly desirable to exploitation had not only had inexpensive but also with high power capacity, electric charge conductive super capacitor carbon soon.
The content of the invention
The invention aims to solve the deficiency of prior art problem, there is provided a kind of preparation method of super capacitor carbon,
Using the corn in agricultural product as raw material, the raw material sources are very abundant and cost is cheap, belong to renewable resource.Corn is former
Material carrys out the good super capacitor carbon of synthesis performance by sorting, purification, carbonization, activation.
To reach above-mentioned purpose, the present invention is implemented according to following technical scheme:
A kind of preparation method of super capacitor carbon, comprises the following steps:
S1, at 25 DEG C of room temperature, dry corn is soaked 10 minutes in aqueous surfactant solution, pulled out latter cool 30 minutes
It is extremely half-dried, obtain the corn of easy degerming skin;
S2, at 25 DEG C of room temperature, with peeling processing equipment the corn in step S1 is removed the peel, to remove institute in corn
The inorganic salts contained, reach the purpose of deliming;
S3, at 25 DEG C of room temperature, broken removing plumule is carried out to the corn after being removed the peel in step S2 with flour mill, is removed beautiful
Contained organic matter in rice, and corn pellet is obtained, reach the purpose of degreasing;
S4, under temperature 60 C, the corn pellet in step S3 is dried 2 hours with drying baker, obtains refined jade
Grain of rice material;
S5, corn pellet is fitted into revolving tubular furnace, under the nitrogen protection of 1 atmospheric pressure, rise temperature 3 per minute
Degree, after room temperature is raised to 100 DEG C, maintain 0.5 hour, remove remnants moisture;
S6, continue to heat up, 2 DEG C of temperature of rise per minute, 300 DEG C are heated to from 100 DEG C, 300 DEG C of constant temperature maintains enter for 1 hour
Row destructive distillation decomposition reaction, low molecular weight volatile point is removed, and reclaim distillate;
S7, continue to heat up, 3 DEG C of temperature of rise per minute, be heated to 400 DEG C from 300 DEG C, maintained 1 hour in 400 DEG C of constant temperature
Destructive distillation decomposition reaction is carried out, removes macromolecule volatile matter, and reclaim distillate;
After S8, decomposition reaction terminate, tube furnace is naturally cooled into room temperature, obtains the presoma that is carbonized;
S9, carbonization presoma is inserted to the obtained porous activated carbon of activated reactor progress priming reaction, then to porous work
Property charcoal is post-processed to obtain super capacitor carbon.
Further, the activation method of the step S9 is that physical activation method prepares super capacitor carbon, is concretely comprised the following steps:
S91, the presoma that is carbonized made from step S8 is fitted into activated reactor, in the case where the nitrogen of 1 atmospheric pressure is protected,
5 degree of temperature of rise per minute, after room temperature is raised to 400 DEG C, is maintained 0.5 hour;
S92, continue to heat up, 3 DEG C of temperature of rise per minute, when being heated to 600 DEG C from 400 DEG C, stop nitrogen, start with every
Minute 0.8m3Speed be passed through vapor to carbonization presoma carry out pre-activate reaction;
S93, continue to heat up, under conditions of continuously vapor is passed through, 3 DEG C of temperature of rise per minute, be heated to from 600 DEG C
800 DEG C, 800 DEG C of constant temperature is maintained 1 hour, and carbonization presoma is activated completely;
After S94, priming reaction terminate, under the nitrogen protection of 1 atmospheric pressure, activated reactor is naturally cooled into room temperature
Activated material is obtained, at 25 DEG C of room temperature, with oxidant with 2:1 weight compares activated material and carries out functional group's doping reaction, obtains
Porous activated carbon I;
S95, at 25 DEG C of room temperature, powder processing is carried out to porous activated carbon I with airflow milling so that porous activated carbon I
Reach the particle diameter and shape need of needs, obtain super capacitor carbon I.
Further, the activation method of the step S9 is that chemical activation method prepares super capacitor carbon, is concretely comprised the following steps:
S91, will be carbonized made from step S8 presoma and caustic alkali are according to weight than 1:2 mixing, it is anti-to load alkaline-resisting activation
Answer in device, be passed through the nitrogen of 1 atmospheric pressure, 5 degree of temperature of rise per minute, after room temperature is raised to 400 DEG C, maintains 0.5 hour, reach
It is uniform to melting mixing;
S92, continue to heat up, be passed through the nitrogen of 1 atmospheric pressure, 5 DEG C of temperature of rise per minute, 600 DEG C be heated to from 400 DEG C
When, 600 DEG C of constant temperature maintains 0.5 hour, reaches pre-activate purpose;
S93, continue to heat up, be passed through the nitrogen of 1 atmospheric pressure, 3 DEG C of temperature of rise per minute, 800 be heated to from 600 DEG C
DEG C, 800 DEG C of constant temperature is maintained 1 hour, and activated material is obtained after reaching activation completely;
After S94, activation terminate, under the nitrogen protection of 1 atmospheric pressure, alkaline-resisting activated reactor is naturally cooled into room
Temperature, carrying out repeatedly washing to activated material with distilled water, to neutrality, drying is porous activated carbon II;
S95, at 25 DEG C of room temperature, powder processing is carried out to porous activated carbon II with airflow milling so that porous activated carbon
II reaches the particle diameter and shape need of needs, obtains super capacitor carbon II.
Preferably, the surfactant in the step S1 is pressed with neopelex and AEO
According to volume ratio 1:1 compounding, then it is configured to the aqueous solution that mass fraction is 0.5%, the surfactant pair with distilled water diluting
There is wetting and scale removal catharsis in corn particle.
Preferably, the oxidant in the step S95 is the aqueous solution for the hydrogen peroxide that mass fraction is 10%, the oxidation
Agent has the function that to adulterate hydroxyl functional group for activated carbon, to improve electrochemistry storage lotus performance.
Compared with prior art, beneficial effects of the present invention are:
Present invention super capacitor carbon inexpensive using corn as Material synthesis first, proposes corn degreasing and takes off first
The pre-treating technology of ash;The carbonization-activation technique that temperature-gradient method removes volatile matter is proposed first;Free from admixture oxygen is proposed first
Change aftertreatment technology.
Process above improves electric conductivity while Large ratio surface is increased, and has good multiplying power property, chemical property
It is close with Japanese South Korea's like product, reach world level, belonged to pioneering at home, carry out high magnification current charge-discharge electricity
When, electrolyte rapidly can adsorb to form electric double layer capacitance as big as possible in electrode interface, so as to avoid declining for specific capacitance
Subtract, realize high current charge-discharge, it is quick that final acquisition has high-specific surface area utilization rate, high stability, high specific capacitance, carrier concurrently
The novel and multifunctional polarizing electrode material of transmission and Reversible Cycle well, the major technique of super capacitor carbon produced by the present invention
Index is:
Using ratio surface >=1800m of super capacitor carbon made from physical activation method2/g;Specific capacity >=160F/g, jolt ramming
Density >=0.30g/cm3, the Ω m of resistivity≤2.0, particle diameter distribution D50≤17 μm, ash content≤0.2%.
Using ratio surface >=1700m of super capacitor carbon made from chemical activation method2/g;Specific capacity >=260F/g, jolt ramming
Density >=0.30g/cm3, the Ω m of resistivity≤2.0, particle diameter distribution D50≤17 μm, ash content≤0.2%.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Fig. 2 is with super capacitor carbon made from physical activation method and the super capacitor carbon of Japanese YP-80 models in the present invention
Charge-discharge magnification curve.
Fig. 3 is with super capacitor carbon made from chemical activation method and the super capacitor carbon of Japanese YP-80 models in the present invention
Charge-discharge magnification curve.
Fig. 4 is super capacitor carbon produced by the present invention and the super capacitor carbon of Japanese YP-80 models respectively in different pressures
Under resistivity curve.
Embodiment
With reference to specific embodiment, the invention will be further described, the illustrative examples and explanation invented herein
For explaining the present invention, but it is not as a limitation of the invention.
As shown in figure 1, being the technological process for preparing the super capacitor carbon of the present invention, enter one below for specific embodiment
Step illustrates the present invention:
Embodiment 1
S1, at 25 DEG C of room temperature, dry corn is soaked 10 minutes in aqueous surfactant solution, pulled out latter cool 30 minutes
It is extremely half-dried, obtain the corn of easy degerming skin;
S2, at 25 DEG C of room temperature, with peeling processing equipment the corn in step S1 is removed the peel, to remove institute in corn
The inorganic salts contained, reach the purpose of deliming;
S3, at 25 DEG C of room temperature, broken removing plumule is carried out to the corn after being removed the peel in step S2 with flour mill, is removed beautiful
Contained organic matter in rice, and corn pellet is obtained, reach the purpose of degreasing;
S4, under temperature 60 C, the corn pellet in step S3 is dried 2 hours with drying baker, obtains refined jade
Grain of rice material;
S5, corn pellet is fitted into revolving tubular furnace, under the nitrogen protection of 1 atmospheric pressure, rise temperature 3 per minute
Degree, after room temperature is raised to 100 DEG C, maintain 0.5 hour, remove remnants moisture;
S6, continue to heat up, 2 DEG C of temperature of rise per minute, 300 DEG C are heated to from 100 DEG C, 300 DEG C of constant temperature maintains enter for 1 hour
Row destructive distillation decomposition reaction, low molecular weight volatile point is removed, and reclaim distillate;
S7, continue to heat up, 3 DEG C of temperature of rise per minute, be heated to 400 DEG C from 300 DEG C, maintained 1 hour in 400 DEG C of constant temperature
Destructive distillation decomposition reaction is carried out, removes macromolecule volatile matter, and reclaim distillate;
After S8, decomposition reaction terminate, tube furnace is naturally cooled into room temperature, obtains the presoma that is carbonized;
S91, the presoma that is carbonized made from step S8 is fitted into activated reactor, in the case where the nitrogen of 1 atmospheric pressure is protected,
5 degree of temperature of rise per minute, after room temperature is raised to 400 DEG C, is maintained 0.5 hour;
S92, continue to heat up, 3 DEG C of temperature of rise per minute, when being heated to 600 DEG C from 400 DEG C, stop nitrogen, start with every
Minute 0.8m3Speed be passed through vapor to carbonization presoma carry out pre-activate reaction;
S93, continue to heat up, under conditions of continuously vapor is passed through, 3 DEG C of temperature of rise per minute, be heated to from 600 DEG C
800 DEG C, 800 DEG C of constant temperature is maintained 1 hour, and carbonization presoma is activated completely;
After S94, priming reaction terminate, under the nitrogen protection of 1 atmospheric pressure, activated reactor is naturally cooled into room temperature
Activated material is obtained, at 25 DEG C of room temperature, with oxidant with 2:1 weight compares activated material and carries out functional group's doping reaction, obtains
Porous activated carbon I;
S95, at 25 DEG C of room temperature, powder processing is carried out to porous activated carbon I with airflow milling so that porous activated carbon I
Reach the particle diameter and shape need of needs, obtain super capacitor carbon I.
Embodiment 2
S1, at 25 DEG C of room temperature, dry corn is soaked 10 minutes in aqueous surfactant solution, pulled out latter cool 30 minutes
It is extremely half-dried, obtain the corn of easy degerming skin;
S2, at 25 DEG C of room temperature, with peeling processing equipment the corn in step S1 is removed the peel, to remove institute in corn
The inorganic salts contained, reach the purpose of deliming;
S3, at 25 DEG C of room temperature, broken removing plumule is carried out to the corn after being removed the peel in step S2 with flour mill, is removed beautiful
Contained organic matter in rice, and corn pellet is obtained, reach the purpose of degreasing;
S4, under temperature 60 C, the corn pellet in step S3 is dried 2 hours with drying baker, obtains refined jade
Grain of rice material;
S5, corn pellet is fitted into revolving tubular furnace, under the nitrogen protection of 1 atmospheric pressure, rise temperature 3 per minute
Degree, after room temperature is raised to 100 DEG C, maintain 0.5 hour, remove remnants moisture;
S6, continue to heat up, 2 DEG C of temperature of rise per minute, 300 DEG C are heated to from 100 DEG C, 300 DEG C of constant temperature maintains enter for 1 hour
Row destructive distillation decomposition reaction, low molecular weight volatile point is removed, and reclaim distillate;
S7, continue to heat up, 3 DEG C of temperature of rise per minute, be heated to 400 DEG C from 300 DEG C, maintained 1 hour in 400 DEG C of constant temperature
Destructive distillation decomposition reaction is carried out, removes macromolecule volatile matter, and reclaim distillate;
After S8, decomposition reaction terminate, tube furnace is naturally cooled into room temperature, obtains the presoma that is carbonized;
S91, will be carbonized made from step S8 presoma and caustic alkali are according to weight than 1:2 mixing, it is anti-to load alkaline-resisting activation
Answer in device, be passed through the nitrogen of 1 atmospheric pressure, 5 degree of temperature of rise per minute, after room temperature is raised to 400 DEG C, maintains 0.5 hour, reach
It is uniform to melting mixing;
S92, continue to heat up, be passed through the nitrogen of 1 atmospheric pressure, 5 DEG C of temperature of rise per minute, 600 DEG C be heated to from 400 DEG C
When, 600 DEG C of constant temperature maintains 0.5 hour, reaches pre-activate purpose;
S93, continue to heat up, be passed through the nitrogen of 1 atmospheric pressure, 3 DEG C of temperature of rise per minute, 800 be heated to from 600 DEG C
DEG C, 800 DEG C of constant temperature is maintained 1 hour, and activated material is obtained after reaching activation completely;
After S94, activation terminate, under the nitrogen protection of 1 atmospheric pressure, alkaline-resisting activated reactor is naturally cooled into room
Temperature, carrying out repeatedly washing to activated material with distilled water, to neutrality, drying is porous activated carbon II;
S95, at 25 DEG C of room temperature, powder processing is carried out to porous activated carbon II with airflow milling so that porous activated carbon
II reaches the particle diameter and shape need of needs, obtains super capacitor carbon II.
To the ratio surface of super capacitor carbon made from embodiment 1 and embodiment 2, specific capacity, tap density, average grain diameter,
Electric conductivity and ash, which grade, measures sign, and specific data are shown in Table 1.
The performance of the super capacitor carbon of table 1
Index | Embodiment 1 | Apply example 2 |
Than surface (m2/g) | 1872 | 1760 |
Specific capacity (F/g) | 160 | 260 |
Tap density (g/cm3) | 0.30 | 0.30 |
Resistivity (Ω m) | 1.2 | 1.3 |
Particle diameter distribution D50 (μm) | 15.0 | 16.5 |
Hui Fen ℅ | 0.2 | 0.2 |
In addition, the super capacitor carbon charge-discharge magnification by super capacitor carbon I made from embodiment 1 and Japanese YP-80 models
Curve is compared, from figure 2 it can be seen that the high rate performance of super capacitor carbon I made from embodiment 1 is under low current conditions
It has been better than or the super capacitor carbon close to Japanese YP-80 models.
By super capacitor carbon II made from embodiment 2 and the super capacitor carbon charge-discharge magnification curve of Japanese YP-80 models
It is compared, from figure 3, it can be seen that the high rate performance of super capacitor carbon II is substantially better than Japanese YP-80 made from embodiment 2
The super capacitor carbon of model.
Furthermore by super capacitor carbon I produced by the present invention or super capacitor carbon II and the super capacitor of Japanese YP-80 models
Carbon tests its resistivity at various pressures respectively, obtains the resistivity curve of super capacitor carbon under different pressures, can from Fig. 4
To find out, its electric conductivity of super capacitor carbon I or super capacitor carbon II produced by the present invention is substantially better than the super of Japanese YP-80 models
Level electric capacity carbon.
Technical scheme is not limited to the limitation of above-mentioned specific embodiment, and every technique according to the invention scheme is done
The technology deformation gone out, each falls within protection scope of the present invention.
Claims (5)
1. a kind of preparation method of super capacitor carbon, it is characterised in that comprise the following steps:
S1, at 25 DEG C of room temperature, dry corn is soaked 10 minutes in the aqueous solution of surfactant, pulls latter cool 30 minutes out extremely
It is half-dried, obtain the corn of easy degerming skin;
S2, at 25 DEG C of room temperature, the corn in step S1 is removed the peel with peeling processing equipment, it is contained to remove in corn
Inorganic salts, reach the purpose of deliming;
S3, at 25 DEG C of room temperature, broken removing plumule is carried out to the corn after being removed the peel in step S2 with flour mill, is removed in corn
Contained organic matter, and corn pellet is obtained, reach the purpose of degreasing;
S4, under temperature 60 C, the corn pellet in step S3 is dried 2 hours with drying baker, obtains refined iblet
Material;
S5, refined corn pellet is fitted into revolving tubular furnace, under the nitrogen protection of 1 atmospheric pressure, rise temperature 3 per minute
Degree, after room temperature is raised to 100 DEG C, maintain 0.5 hour, remove remnants moisture;
S6, continue to heat up, 2 DEG C of temperature of rise per minute, 300 DEG C are heated to from 100 DEG C, 300 DEG C of constant temperature maintains done for 1 hour
Decomposition reaction is evaporated, removes low molecular weight volatile point, and reclaim distillate;
S7, continue to heat up, 3 DEG C of temperature of rise per minute is heated to 400 DEG C from 300 DEG C, maintains carry out within 1 hour in 400 DEG C of constant temperature
Destructive distillation decomposition reaction, macromolecule volatile matter is removed, and reclaim distillate;
After S8, decomposition reaction terminate, tube furnace is naturally cooled into room temperature, obtains the presoma that is carbonized;
S9, carbonization presoma is inserted to the obtained porous activated carbon of activated reactor progress priming reaction, then to porous activated carbon
Post-processed to obtain super capacitor carbon.
2. the preparation method of super capacitor carbon according to claim 1, it is characterised in that:The activation method of the step S9
Super capacitor carbon is prepared for physical activation method, is concretely comprised the following steps:
S91, the presoma that is carbonized made from step S8 is fitted into activated reactor, in the case where the nitrogen of 1 atmospheric pressure is protected, every point
Clock raises 5 degree of temperature, after room temperature is raised to 400 DEG C, maintains 0.5 hour;
S92, continue to heat up, 3 DEG C of temperature of rise per minute, when being heated to 600 DEG C from 400 DEG C, stop nitrogen, start with per minute
0.8m3Speed be passed through vapor to carbonization presoma carry out pre-activate reaction;
S93, continue to heat up, under conditions of continuously vapor is passed through, 3 DEG C of temperature of rise per minute, 800 are heated to from 600 DEG C
DEG C, 800 DEG C of constant temperature is maintained 1 hour, and carbonization presoma is activated completely;
After S94, priming reaction terminate, under the nitrogen protection of 1 atmospheric pressure, activated reactor is naturally cooled into room temperature and obtained
Activated material, at 25 DEG C of room temperature, with oxidant with 2:1 weight compares activated material and carries out functional group's doping reaction, obtains porous
Activated carbon I;
S95, at 25 DEG C of room temperature, powder processing is carried out to porous activated carbon I with airflow milling so that porous activated carbon I reaches
The particle diameter and shape need needed, obtains super capacitor carbon I.
3. the preparation method of super capacitor carbon according to claim 1, it is characterised in that:The activation method of the step S9
Super capacitor carbon is prepared for chemical activation method, is concretely comprised the following steps:
S91, will be carbonized made from step S8 presoma and caustic alkali are according to weight than 1:2 mixing, load alkaline-resisting activated reactor
In, the nitrogen of 1 atmospheric pressure is passed through, 5 degree of temperature of rise per minute, after room temperature is raised to 400 DEG C, maintains 0.5 hour, reaches molten
Melt well mixed;
S92, continue to heat up, be passed through the nitrogen of 1 atmospheric pressure, it is per minute to raise 5 DEG C of temperature, when being heated to 600 DEG C from 400 DEG C,
600 DEG C of constant temperature maintains 0.5 hour, reaches pre-activate purpose;
S93, continue to heat up, be passed through the nitrogen of 1 atmospheric pressure, 3 DEG C of temperature of rise per minute, 800 DEG C be heated to from 600 DEG C, perseverance
800 DEG C of temperature is maintained 1 hour, and activated material is obtained after reaching activation completely;
After S94, activation terminate, under the nitrogen protection of 1 atmospheric pressure, alkaline-resisting activated reactor is naturally cooled into room temperature, used
Distilled water carries out repeatedly washing to activated material, and, to neutrality, drying is porous activated carbon II;
S95, at 25 DEG C of room temperature, powder processing is carried out to porous activated carbon II with airflow milling so that porous activated carbon II reaches
To the particle diameter and shape need of needs, super capacitor carbon II is obtained.
4. the preparation method of super capacitor carbon according to claim 1, it is characterised in that:Live on surface in the step S1
Property agent neopelex and AEO according to volume ratio 1:1 compounding, is then matched somebody with somebody with distilled water diluting
The aqueous solution that mass fraction is 0.5% is made.
5. the preparation method of super capacitor carbon according to claim 2, it is characterised in that:Oxidation in the step S95
Agent is the aqueous solution for the hydrogen peroxide that mass fraction is 10%.
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CN108975328A (en) * | 2018-09-25 | 2018-12-11 | 河南师范大学 | A kind of two steps method that carbonization prepares the biomass porous carbon material of nitrogen oxygen codope in advance |
CN109368636A (en) * | 2018-12-07 | 2019-02-22 | 武汉工程大学 | A kind of preparation method of the classifying porous doping carbon material of modified |
CN111137886A (en) * | 2019-11-19 | 2020-05-12 | 南京工程学院 | Method for preparing electrode material by aquatic plant |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108975328A (en) * | 2018-09-25 | 2018-12-11 | 河南师范大学 | A kind of two steps method that carbonization prepares the biomass porous carbon material of nitrogen oxygen codope in advance |
CN108975328B (en) * | 2018-09-25 | 2021-07-20 | 河南师范大学 | Method for preparing nitrogen-oxygen co-doped biomass porous carbon material through two-step pre-carbonization |
CN109368636A (en) * | 2018-12-07 | 2019-02-22 | 武汉工程大学 | A kind of preparation method of the classifying porous doping carbon material of modified |
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