CN108002360A - A kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor - Google Patents
A kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor Download PDFInfo
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- CN108002360A CN108002360A CN201711240122.8A CN201711240122A CN108002360A CN 108002360 A CN108002360 A CN 108002360A CN 201711240122 A CN201711240122 A CN 201711240122A CN 108002360 A CN108002360 A CN 108002360A
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- shrimp
- crab shells
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- electrode material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The present invention relates to a kind of preparation method of electrode material for super capacitor, and in particular to a kind of preparation method based on shrimp and crab shells biomass carbon electrode material for super capacitor.This method includes shrimp and crab shells pre-treatment, once carbonizes, activates, secondary charing, carbon source of the present invention using shrimp and crab shells as electrode material for super capacitor, is a kind of absorbent charcoal material prepared using marine biomass；The specific surface area for the electrode carbon material that the present invention is prepared is high, specific capacitance is high, and the present invention possesses energy-saving and emission-reduction, low-carbon environment-friendly, the more low advantage of requirement to equipment.
Description
Technical field
The present invention relates to a kind of preparation method of electrode material for super capacitor, and in particular to one kind is based on shrimp and crab shells biology
The preparation method of matter charcoal super capacitor electrode material.
Background technology
It is estimated that the shrimp discarded after annual edible, crab shell there are about hundreds of thousands ton, this not only to waste of resources is caused,
Pollution is brought to living environment.Therefore, how the high-valued marine organisms waste resources such as shrimp, crab shell of developing have caused research work
The extensive concern of person, for example, using shrimp shell crab shell as raw material, can prepare the derivatives such as chitin and chitosan, and utilize chitosan
Spongy ordered porous nano adsorption material is can be made into, but utilization shrimp and crab shells extraction chitosan is of high cost, complex process.
The content of the invention
In order to solve the problems, such as the wasting of resources, the present invention prepares biomass carbon material using discarded shrimp, crab shell, is applied to
Electrode of super capacitor.The present invention provides a kind of preparation method based on shrimp crab biomass carbon electrode material for super capacitor,
This method includes shrimp and crab shells pre-treatment, once carbonizes, activates, secondary charing.
A kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor, comprises the following steps that：
1) pre-process：Shrimp and crab shells are cleaned up, are placed in 60-100 DEG C of thermostatic drying chamber dry 6-10h, and using micro-
Nano grinder smashes, and crosses 500-800 mesh sieves；
2) once carbonize：Pretreated shrimp and crab shells powder in step 1) is placed in tube furnace and is carbonized, carbonization temperature
600-1000 DEG C, carbonization time 2-5h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition；
3) activate：Shrimp and crab shells powder after once being carbonized in step 2) is cleaned into 1-3h with 20-50%KOH in 50-70 DEG C
Activated, 15h is cleaned in 60 DEG C using the HCl of 1-5mol/L, removes remaining impurity, and be washed with distilled water, filtered
Precipitation is collected, the shrimp and crab shells powder being dried in vacuo after being activated；
4) secondary charing：Shrimp and crab shells powder after activation in step 3) is placed in secondary charing, carbonization temperature in tube furnace
300-500 DEG C, carbonization time 1-4h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition；With steaming after charing
Distilled water is washed for several times, the dry 6-10h in 60-100 DEG C of thermostatic drying chamber, you can obtain the super capacitor using shrimp and crab shells as carbon source
Device electrode material.
Preferably, shrimp shell is mixed with the weight ratio of crab shell for arbitrary proportion in shrimp and crab shells in the step 1).
Preferably, the drying temperature in the step 1) is 80 DEG C.
Preferably, the carbonization temperature in step 2) is 800 DEG C.
Preferably, the concentration of the KOH in the step 3) is 30%, the volumetric usage of the KOH is after once carbonizing
3 times of shrimp and crab shells powder weight, units/ml/g.
Preferably, the concentration of the HCl in the step 3) is 3mol/L, the volumetric usage of the HCl is once to carbonize
2 times of shrimp and crab shells powder weight afterwards, units/ml/g.
Preferably, the carbonization temperature in the step 4) is 400 DEG C.
As advantage, the drying temperature in the step 4) is 80 DEG C.
Carbon source of the present invention using shrimp and crab shells as electrode material for super capacitor, is a kind of work prepared using marine biomass
Property Carbon Materials.The specific surface area for the electrode carbon material that the present invention is prepared is high, specific capacitance is high, and the present invention possesses energy saving subtract
Row, low-carbon environment-friendly, the more low advantage of requirement to equipment.
Embodiment
Embodiment 1
1) pre-process：Shrimp shell 1KG, crab shell 1KG are cleaned up, are placed in 60 DEG C of thermostatic drying chambers dry 10h, and use
Micro-nano pulverizer smashes, and crosses 800 mesh sieves, obtains shrimp and crab shells powder 1000g；
2) once carbonize：Pretreated shrimp and crab shells powder in step 1) is placed in tube furnace and is carbonized, carbonization temperature
600 DEG C, carbonization time 5h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, shrimp and crab shells after must carbonizing
Powder 300g；
3) activate：Shrimp and crab shells powder after once being carbonized in step 2) is cleaned in 70 DEG C with 20%KOH 900mL 1h into
Row activation, cleans 15h in 60 DEG C using the HCl 600mL of 5mol/L, removes remaining impurity, and be washed with distilled water, mistake
Precipitation is collected in filter, the shrimp and crab shells powder 250g being dried in vacuo after being activated；
4) secondary charing：Shrimp after activation in step 3), crab shell powder are placed in secondary charing, carbonization temperature in tube furnace
500 DEG C, carbonization time 1h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition；With distillation washing after charing
Wash for several times, the dry 6h in 100 DEG C of thermostatic drying chambers, you can obtain the electrode material for super capacitor using shrimp and crab shells as carbon source.
Its specific surface area and specific volume are measured, the results are shown in Table 1.
Table 1
| Specific surface area (m2/g) | Specific volume (F/g) |
| 1200 | 300 |
Embodiment 2
1) pre-process：Shrimp shell 1.5KG, crab shell 1.5KG are cleaned up, are placed in 100 DEG C of thermostatic drying chambers dry 6h, and
Smashed using micro-nano pulverizer, cross 500 mesh sieves, obtain shrimp and crab shells powder 1350g；
2) once carbonize：Pretreated shrimp and crab shells powder in step 1) is placed in tube furnace and is carbonized, carbonization temperature
1000 DEG C, carbonization time 2h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, shrimp and crab shells after must carbonizing
Powder 400g；
3) activate：Shrimp and crab shells powder after once being carbonized in step 2) is cleaned in 50 DEG C with 50%KOH 1200mL 3h into
Row activation, cleans 15h in 60 DEG C using the HCl 800mL of 3mol/L, removes remaining impurity, and be washed with distilled water, mistake
Precipitation is collected in filter, the shrimp and crab shells powder 320g being dried in vacuo after being activated；
4) secondary charing：Shrimp and crab shells powder after activation in step 3) is placed in secondary charing in tube furnace, carbonization temperature 300
DEG C, carbonization time 4h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition；It is washed with distilled water after charing
For several times, the dry 8h in 80 DEG C of thermostatic drying chambers, you can obtain the electrode material for super capacitor using shrimp and crab shells as carbon source.
Its specific surface area and specific volume are measured, the results are shown in Table 2.
Table 2
| Specific surface area (m2/g) | Specific volume (F/g) |
| 1350 | 350 |
Embodiment 3
1) pre-process：Shrimp shell 2KG, crab shell 1KG are cleaned up, are placed in 80 DEG C of thermostatic drying chambers dry 8h, and use
Micro-nano pulverizer smashes, and crosses 700 mesh sieves, obtains shrimp and crab shells powder 1300g；
2) once carbonize：Pretreated shrimp and crab shells powder in step 1) is placed in tube furnace and is carbonized, carbonization temperature
800 DEG C, carbonization time 4h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, shrimp and crab shells after must carbonizing
Powder 380g；
3) activate：Shrimp and crab shells powder after once being carbonized in step 2) is cleaned in 70 DEG C with 30%KOH 1140mL 1h into
Row activation, cleans 15h in 60 DEG C using the HCl 760mL of 3mol/L, removes remaining impurity, and be washed with distilled water, mistake
Precipitation is collected in filter, the shrimp and crab shells powder 280g being dried in vacuo after being activated；
4) secondary charing：Shrimp after activation in step 3), crab shell powder are placed in secondary charing, carbonization temperature in tube furnace
400 DEG C, carbonization time 3h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition；With distillation washing after charing
Wash for several times, the dry 8h in 80 DEG C of thermostatic drying chambers, you can obtain the electrode material for super capacitor using shrimp and crab shells as carbon source.
Its specific surface area and specific volume are measured, the results are shown in Table 3.
Table 3
| Specific surface area (m2/g) | Specific volume (F/g) |
| 1600 | 420 |
Embodiment 4
1) pre-process：Shrimp shell 1KG, crab shell 3KG are cleaned up, are placed in 90 DEG C of thermostatic drying chambers dry 7h, and use
Micro-nano pulverizer smashes, and crosses 800 mesh sieves, obtains shrimp and crab shells powder 1800g；
2) once carbonize：Pretreated shrimp and crab shells powder in step 1) is placed in tube furnace and is carbonized, carbonization temperature
900 DEG C, carbonization time 3h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, shrimp and crab shells after must carbonizing
Powder 400g；
3) activate：Shrimp and crab shells powder after once being carbonized in step 2) is cleaned in 60 DEG C with 25%KOH 1200mL 2h into
Row activation, cleans 15h in 60 DEG C using the HCl 800mL of 4mol/L, removes remaining impurity, and be washed with distilled water, mistake
Precipitation is collected in filter, the shrimp and crab shells powder 300g being dried in vacuo after being activated；
4) secondary charing：Shrimp and crab shells powder after activation in step 3) is placed in secondary charing in tube furnace, carbonization temperature 400
DEG C, carbonization time 4h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition；It is washed with distilled water after charing
For several times, the dry 8h in 100 DEG C of thermostatic drying chambers, you can obtain the electrode material for super capacitor using shrimp and crab shells as carbon source.
Its specific surface area and specific volume are measured, the results are shown in Table 4.
Table 4
| Specific surface area (m2/g) | Specific volume (F/g) |
| 1500 | 380 |
Embodiment 5
1) pre-process：Shrimp shell 3KG, crab shell 5KG are cleaned up, are placed in 100 DEG C of thermostatic drying chambers dry 6h, and use
Micro-nano pulverizer smashes, and crosses 550 mesh sieves, obtains shrimp and crab shells powder 4000g；
2) once carbonize：Pretreated shrimp and crab shells powder in step 1) is placed in tube furnace and is carbonized, carbonization temperature
800 DEG C, carbonization time 2.5h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, shrimp crab after must carbonizing
Shell powder 800g；
3) activate：Shrimp and crab shells powder after once being carbonized in step 2) is cleaned in 65 DEG C with 30%KOH 2400mL 3h into
Row activation, cleans 15h in 60 DEG C using the HCl 1600mL of 2mol/L, removes remaining impurity, and be washed with distilled water, mistake
Precipitation is collected in filter, the shrimp and crab shells powder 680g being dried in vacuo after being activated；
4) secondary charing：Shrimp and crab shells powder after activation in step 3) is placed in secondary charing in tube furnace, carbonization temperature 350
DEG C, carbonization time 3h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition；It is washed with distilled water after charing
For several times, the dry 8h in 80 DEG C of thermostatic drying chambers, you can obtain the electrode material for super capacitor using shrimp and crab shells as carbon source.
Its specific surface area and specific volume are measured, the results are shown in Table 5.
Table 5
| Specific surface area (m2/g) | Specific volume (F/g) |
| 1500 | 400 |
This place embodiment is in place of the claimed non-limit of technical scope midrange and in embodiment technology
The new technical solution formed is replaced on an equal basis to single or multiple technical characteristics in scheme, equally all in application claims
In the range of protection；At the same time the present invention program it is all enumerate or unrequited embodiment in, in the same embodiment each
Parameter is merely representative of an example (i.e. a kind of feasible scheme) for its technical solution, and between parameters and is not present stringent
Cooperation and qualified relation, wherein each parameter can be replaced mutually when stating and asking without prejudice to axiom and the present invention, special declaration
Except.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, further includes
Formed technical solution is combined by above technical characteristic.The above is the embodiment of the present invention, should be referred to
Go out, for those skilled in the art, without departing from the principle of the present invention, can also make some
Improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (8)
1. a kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor, it is characterised in that comprise the following steps：
1) pre-process：Shrimp and crab shells are cleaned up, are placed in 60-100 DEG C of thermostatic drying chamber dry 6-10h, and using micro-nano
Pulverizer smashes, and crosses 500-800 mesh sieves；
2) once carbonize：Pretreated shrimp and crab shells powder in step 1) is placed in tube furnace and is carbonized, carbonization temperature 600-
1000 DEG C, carbonization time 2-5h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition；
3) activate：The shrimp and crab shells powder after once carbonizing in step 2) is cleaned 1-3h in 50-70 DEG C with 20-50%KOH to carry out
Activation, cleans 15h in 60 DEG C using the HCl of 1-5mol/L, removes remaining impurity, and is washed with distilled water, and is collected by filtration
Precipitation, the shrimp and crab shells powder being dried in vacuo after being activated；
4) secondary charing：Shrimp and crab shells powder after activation in step 3) is placed in secondary charing in tube furnace, carbonization temperature 300-500
DEG C, carbonization time 1-4h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition；With distillation washing after charing
Wash for several times, the dry 6-10h in 60-100 DEG C of thermostatic drying chamber, you can obtain the electrode of super capacitor using shrimp and crab shells as carbon source
Material.
2. a kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor according to claim 1, it is special
Sign is in the shrimp and crab shells in the step 1) that shrimp shell is mixed with the weight ratio of crab shell for arbitrary proportion.
3. a kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor according to claim 1, it is special
Sign is that the drying temperature in the step 1) is 80 DEG C.
4. a kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor according to claim 1, it is special
Sign is that the carbonization temperature in step 2) is 800 DEG C.
5. a kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor according to claim 1, it is special
Sign is that the concentration of the KOH in the step 3) is 30%, and the volumetric usage of the KOH is shrimp and crab shells powder weight after once charing
3 times, units/ml/g.
6. a kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor according to claim 1, it is special
Sign is that the concentration of the HCl in the step 3) is 3mol/L, and the volumetric usage of the HCl is shrimp and crab shells powder weight after once charing
2 times of amount, units/ml/g.
7. a kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor according to claim 1, it is special
Sign is that the carbonization temperature in the step 4) is 400 DEG C.
8. a kind of preparation based on shrimp and crab shells biomass carbon electrode material for super capacitor according to claim 1, it is special
Sign is that the drying temperature in the step 4) is 80 DEG C.
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| CN110155979A (en) * | 2019-04-09 | 2019-08-23 | 中国海洋大学 | It is a kind of regulate and control Marine fishbone class biological carbon Heteroatom doping amount method and its store up sodium device application |
| CN110327898A (en) * | 2019-07-01 | 2019-10-15 | 河南城建学院 | A kind of shrimp shell base magnetism multi-stage porous carbon surface imprinted material and its preparation method and application |
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Application publication date: 20180508 |