CN108010749A - A kind of preparation method based on kelp biomass charcoal super capacitor electrode material - Google Patents

A kind of preparation method based on kelp biomass charcoal super capacitor electrode material Download PDF

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Publication number
CN108010749A
CN108010749A CN201711242181.9A CN201711242181A CN108010749A CN 108010749 A CN108010749 A CN 108010749A CN 201711242181 A CN201711242181 A CN 201711242181A CN 108010749 A CN108010749 A CN 108010749A
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China
Prior art keywords
kelp
electrode material
super capacitor
preparation
charing
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CN201711242181.9A
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Chinese (zh)
Inventor
纪丽丽
宋文东
郭健
蔡璐
王亚宁
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Zhejiang Ocean University ZJOU
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Zhejiang Ocean University ZJOU
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Priority to CN201711242181.9A priority Critical patent/CN108010749A/en
Publication of CN108010749A publication Critical patent/CN108010749A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/44Raw materials therefor, e.g. resins or coal
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/34Carbon-based characterised by carbonisation or activation of carbon
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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  • 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 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 kelp biomass charcoal super capacitor electrode material.The preparation method include pre-treatment, once carbonize, activate, it is secondary charing and etc., the present invention using kelp be used as the carbon source of electrode material for super capacitor, be it is a kind of using marine biomass preparation absorbent charcoal material;The electrode carbon material that the present invention is prepared has the advantages that specific surface area is high, specific capacitance is high, while the method for the present invention energy-saving and emission-reduction, low-carbon environment-friendly, the requirement to equipment are lower.

Description

A kind of preparation method based on kelp biomass charcoal super capacitor electrode material
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 kelp biomass The preparation method of charcoal super capacitor electrode material.
Background technology
Ultracapacitor is a kind of a kind of new fast energy storage device between ordinary capacitor and chemical cell, It is widely regarded as a kind of practical low-carbon energy storage device.The performance of ultracapacitor depends primarily upon electrode material, commonly uses The electrode material of ultracapacitor have carbon material, transition metal oxide, hydroxide and conducting polymer etc., wherein carbon materials Material is with its good charging and discharging capabilities by researcher Depth Study.Activated carbon is most common carbon material, since its is opposite In some other carbon material manufacturing cost is low, technique is simple, industrialized production can be carried out, and its be suitable as ultracapacitor Material.But the raw material of existing high grade activated carbon is mainly timber and coal, this does not meet today's society for sustained development Demand, therefore using biomass prepare activated carbon be development trend.In recent years, many researchers are all in research biology The preparation of activated carbon, has using catkin maize peel etc., but energy storage is relatively low, the specific surface area for the carbon material produced it is relatively low and Energy storage effect is poor.
The content of the invention
Existing in the prior art in order to solve the problems, such as, the present invention provides one kind to be based on kelp biomass charcoal super capacitor The preparation method of electrode material, the carbon source of electrode material for super capacitor prepared by the present invention is kelp, is that one kind utilizes ocean Absorbent charcoal material prepared by biomass;The specific surface area for the electrode carbon material that the present invention is prepared is high, specific capacitance is high, Er Qieben Inventive method more energy-saving and emission-reduction, low-carbon environment-friendly, the requirement to equipment are lower.
A kind of preparation method based on kelp biomass charcoal super capacitor electrode material, including pre-treatment, once charing, Activation, secondary charing, comprise the following steps that:
1) pre-treatment
By Fresh Laminaria Japonica after ultrasonic cleaning is clean, dry 6-10h is placed in 60-100 DEG C of thermostatic drying chamber, and carried out Coarse crushing;
2) once carbonize
Kelp Powder after pre-treatment in step 1) is placed in tube furnace and is carbonized, 500-1100 DEG C of carbonization temperature, charcoal Change time 2-6h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition;
3) activate
The Kelp Powder after once carbonizing in step 2) is cleaned 1-3h in 50-70 DEG C with 20-50%KOH to be activated, 15h is cleaned in 60 DEG C using the HCl of 1-5mol/L, removes remaining impurity, and is washed with distilled water, precipitation is collected by filtration, The kelp being dried in vacuo after being activated;
4) secondary charing
Kelp Powder after activation in step 3) is placed in secondary charing in tube furnace, 300-500 DEG C of carbonization temperature, during charing Between 1-5h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition, be washed with distilled water after charing for several times, Dry 6-10h in 60-100 DEG C of thermostatic drying chamber, you can obtain the electrode material for super capacitor using kelp as carbon source.
Preferably, the drying temperature in the step 1) is 80 DEG C.
Preferably, the carbonization temperature in the step 2) is 700 DEG C.
Preferably, the KOH concentration in the step 3) is 30%, the volumetric usage of the KOH is shrimp after once charing 3 times of crab shell 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.
Preferably, the drying temperature in the step 4) is 80 DEG C.
The present invention, as the carbon source of electrode material for super capacitor, is a kind of work prepared using marine biomass using kelp Property Carbon Materials;The electrode carbon material that the present invention is prepared has the advantages that specific surface area is high, specific capacitance is high, while present invention side Method energy-saving and emission-reduction, low-carbon environment-friendly, the requirement to equipment are lower.
Embodiment
Embodiment 1
1) pre-treatment
By Fresh Laminaria Japonica 1KG after ultrasonic cleaning is clean, dry 10h is placed in 60 DEG C of thermostatic drying chambers, and is carried out thick Crush, obtain Kelp Powder 200g;
2) once carbonize
Kelp Powder after pre-treatment in step 1) is placed in tube furnace and is carbonized, 1100 DEG C of carbonization temperature, during charing Between 2h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, obtain once charing after Kelp Powder 40g;
3) activate
The Kelp Powder after once carbonizing in step 2) is cleaned 1h in 70 DEG C with 20%KOH 120mL to be activated, is adopted 15h is cleaned in 60 DEG C with the HCl 80mL of 1mol/L, removes remaining impurity, and is washed with distilled water, precipitation is collected by filtration, The kelp 30g being dried in vacuo after being activated;
4) secondary charing
Kelp Powder after activation in step 3) is placed in secondary charing in tube furnace, 500 DEG C of carbonization temperature, carbonization time 1h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition, is washed with distilled water for several times after charing, at 100 DEG C Dry 6h in thermostatic drying chamber, you can obtain the electrode material for super capacitor 20g using kelp as carbon source.Measure its specific surface area And specific capacitance, the results are shown in Table 1.
Table 1
Specific surface area (m2/g) Specific capacitance (F/g)
856 220
Embodiment 2
1) pre-treatment
By Fresh Laminaria Japonica 1.5KG after ultrasonic cleaning is clean, dry 6h is placed in 100 DEG C of thermostatic drying chambers, and carried out Coarse crushing, obtains Kelp Powder 250g;
2) once carbonize
Kelp Powder after pre-treatment in step 1) is placed in tube furnace and is carbonized, 500 DEG C of carbonization temperature, carbonization time 6h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, obtain once charing after Kelp Powder 50g;
3) activate
The Kelp Powder after once carbonizing in step 2) is cleaned 2h in 60 DEG C with 40%KOH 150mL to be activated, is adopted 15h is cleaned in 60 DEG C with the HCl 100mL of 2mol/L, removes remaining impurity, and is washed with distilled water, it is heavy to be collected by filtration Form sediment, the kelp 38g being dried in vacuo after being activated;
4) secondary charing
Kelp Powder after activation in step 3) is placed in secondary charing in tube furnace, 300 DEG C of carbonization temperature, carbonization time 5h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition, is washed with distilled water for several times after charing, at 60 DEG C Dry 10h in thermostatic drying chamber, you can obtain the electrode material for super capacitor 25g using kelp as carbon source.Measure it and compare surface Product and specific capacitance, the results are shown in Table 2.
Table 2
Specific surface area (m2/g) Specific capacitance (F/g)
683 180
Embodiment 3
1) pre-treatment
By Fresh Laminaria Japonica 2KG after ultrasonic cleaning is clean, dry 8h is placed in 80 DEG C of thermostatic drying chambers, and carry out coarse powder It is broken, obtain Kelp Powder 300g;
2) once carbonize
Kelp Powder after pre-treatment in step 1) is placed in tube furnace and is carbonized, 700 DEG C of carbonization temperature, carbonization time 4h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, obtain once charing after Kelp Powder 60g;
3) activate
The Kelp Powder after once carbonizing in step 2) is cleaned 3h in 50 DEG C with 30%KOH 180mL to be activated, is adopted 15h is cleaned in 60 DEG C with the HCl 120mL of 3mol/L, removes remaining impurity, and is washed with distilled water, it is heavy to be collected by filtration Form sediment, the kelp 45g being dried in vacuo after being activated;
4) secondary charing
Kelp Powder after activation in step 3) is placed in secondary charing in tube furnace, 400 DEG C of carbonization temperature, carbonization time 2h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition, is washed with distilled water for several times after charing, at 80 DEG C Dry 7h in thermostatic drying chamber, you can obtain the electrode material for super capacitor 32g using kelp as carbon source.Measure its specific surface area And specific capacitance, the results are shown in Table 3.
Table 3
Specific surface area (m2/g) Specific capacitance (F/g)
1230 250
Embodiment 4
1) pre-treatment
By Fresh Laminaria Japonica 2.5KG after ultrasonic cleaning is clean, dry 8h is placed in 70 DEG C of thermostatic drying chambers, and is carried out thick Crush, obtain Kelp Powder 350g;
2) once carbonize
Kelp Powder after pre-treatment in step 1) is placed in tube furnace and is carbonized, 600 DEG C of carbonization temperature, carbonization time 5h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, obtain once charing after Kelp Powder 80g;
3) activate
The Kelp Powder after once carbonizing in step 2) is cleaned 3h in 70 DEG C with 20%KOH 240mL to be activated, is adopted 15h is cleaned in 60 DEG C with the HCl 160mL of 5mol/L, removes remaining impurity, and is washed with distilled water, it is heavy to be collected by filtration Form sediment, the kelp 65g being dried in vacuo after being activated;
4) secondary charing
Kelp Powder after activation in step 3) is placed in secondary charing in tube furnace, 400 DEG C of carbonization temperature, carbonization time 4h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition, is washed with distilled water for several times after charing, at 65 DEG C Dry 10h in thermostatic drying chamber, you can obtain the electrode material for super capacitor 50g using kelp as carbon source.Measure it and compare surface Product and specific capacitance, the results are shown in Table 4.
Table 4
Specific surface area (m2/g) Specific capacitance (F/g)
960 230
Embodiment 5
1) pre-treatment
By Fresh Laminaria Japonica 3KG after ultrasonic cleaning is clean, dry 7h is placed in 90 DEG C of thermostatic drying chambers, and carry out coarse powder It is broken, obtain Kelp Powder 450g;
2) once carbonize
Kelp Powder after pre-treatment in step 1) is placed in tube furnace and is carbonized, 650 DEG C of carbonization temperature, carbonization time 6h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition, obtain once charing after Kelp Powder 100g;
3) activate
The Kelp Powder after once carbonizing in step 2) is cleaned 3h in 60 DEG C with 50%KOH 300mL to be activated, is adopted 15h is cleaned in 60 DEG C with the HCl 200mL of 5mol/L, removes remaining impurity, and is washed with distilled water, it is heavy to be collected by filtration Form sediment, the kelp 80g being dried in vacuo after being activated;
4) secondary charing
Kelp Powder after activation in step 3) is placed in secondary charing in tube furnace, 500 DEG C of carbonization temperature, carbonization time 2h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition, is washed with distilled water for several times after charing, at 100 DEG C Dry 6h in thermostatic drying chamber, you can obtain the electrode material for super capacitor 65g using kelp as carbon source.Measure its specific surface area And specific capacitance, the results are shown in Table 5.
Table 5
Specific surface area (m2/g) Specific capacitance (F/g)
1020 230
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 (7)

1. a kind of preparation method based on kelp biomass charcoal super capacitor electrode material, it is characterised in that including following step Suddenly:
1) pre-treatment
By Fresh Laminaria Japonica after ultrasonic cleaning is clean, dry 6-10h is placed in 60-100 DEG C of thermostatic drying chamber, and carry out coarse powder It is broken;
2) once carbonize
Kelp Powder after pre-treatment in step 1) is placed in tube furnace and is carbonized, 500-1100 DEG C of carbonization temperature, during charing Between 2-6h, inert gas N2Flow be 100mL/min, 10 DEG C/min of the rate of heat addition;
3) activate
The Kelp Powder after once carbonizing in step 2) is cleaned 1-3h in 50-70 DEG C with 20-50%KOH to be activated, is used The HCl of 1-5mol/L cleans 15h in 60 DEG C, removes remaining impurity, and is washed with distilled water, and precipitation, vacuum is collected by filtration The kelp being dried to obtain after activation;
4) secondary charing
Kelp Powder after activation in step 3) is placed in secondary charing in tube furnace, 300-500 DEG C of carbonization temperature, carbonization time 1- 5h, inert gas N2Flow be 50mL/min, 10 DEG C/min of the rate of heat addition, is washed with distilled water after charing for several times, in 60- Dry 6-10h in 100 DEG C of thermostatic drying chambers, you can obtain the electrode material for super capacitor using kelp as carbon source.
2. a kind of preparation method based on kelp biomass charcoal super capacitor electrode material according to claim 1, its The drying temperature being characterized in that in the step 1) is 80 DEG C.
3. a kind of preparation method based on kelp biomass charcoal super capacitor electrode material according to claim 1, its The carbonization temperature being characterized in that in the step 2) is 700 DEG C.
4. a kind of preparation method based on kelp biomass charcoal super capacitor electrode material according to claim 1, its The KOH concentration being characterized in that 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.
5. a kind of preparation method based on kelp biomass charcoal super capacitor electrode material according to claim 1, its The concentration for the HCL being characterized in that in the step 3) is 3mol/L, and the volumetric usage of the HCl is shrimp and crab shells powder after once charing 2 times of weight, units/ml/g.
6. a kind of preparation method based on kelp biomass charcoal super capacitor electrode material according to claim 1, its The carbonization temperature being characterized in that in the step 4) is 400 DEG C.
7. a kind of preparation method based on kelp biomass charcoal super capacitor electrode material according to claim 1, its The drying temperature being characterized in that in the step 4) is 80 DEG C.
CN201711242181.9A 2017-11-30 2017-11-30 A kind of preparation method based on kelp biomass charcoal super capacitor electrode material Pending CN108010749A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109192984A (en) * 2018-08-24 2019-01-11 宁波科力安新能源技术有限公司 A kind of lithium battery
CN109659144A (en) * 2018-12-06 2019-04-19 桂林理工大学 A method of high pressure water system electrode material for super capacitor is prepared using bagasse
CN109928392A (en) * 2019-05-08 2019-06-25 哈尔滨理工大学 A kind of preparation based on biomass carbon electrode material for super capacitor derived from elm money
CN111908443A (en) * 2020-06-24 2020-11-10 西安理工大学 Preparation method of self-doped porous carbon

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Publication number Priority date Publication date Assignee Title
CN105858651A (en) * 2016-03-31 2016-08-17 覃淑兰 A preparing method of activated carbon
CN107285315A (en) * 2017-08-08 2017-10-24 中国林业科学研究院林产化学工业研究所 A kind of adjustable aperture obtains soluble alginate base super capacitor active carbon material and one step charing preparation method

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CN105858651A (en) * 2016-03-31 2016-08-17 覃淑兰 A preparing method of activated carbon
CN107285315A (en) * 2017-08-08 2017-10-24 中国林业科学研究院林产化学工业研究所 A kind of adjustable aperture obtains soluble alginate base super capacitor active carbon material and one step charing preparation method

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109192984A (en) * 2018-08-24 2019-01-11 宁波科力安新能源技术有限公司 A kind of lithium battery
CN109192984B (en) * 2018-08-24 2022-04-29 宁波科力安新能源技术有限公司 Lithium battery
CN109659144A (en) * 2018-12-06 2019-04-19 桂林理工大学 A method of high pressure water system electrode material for super capacitor is prepared using bagasse
CN109928392A (en) * 2019-05-08 2019-06-25 哈尔滨理工大学 A kind of preparation based on biomass carbon electrode material for super capacitor derived from elm money
CN111908443A (en) * 2020-06-24 2020-11-10 西安理工大学 Preparation method of self-doped porous carbon

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