CN109671573A - A kind of preparation method of super capacitor material and products thereof and application - Google Patents
A kind of preparation method of super capacitor material and products thereof and application Download PDFInfo
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- CN109671573A CN109671573A CN201811627198.0A CN201811627198A CN109671573A CN 109671573 A CN109671573 A CN 109671573A CN 201811627198 A CN201811627198 A CN 201811627198A CN 109671573 A CN109671573 A CN 109671573A
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- Prior art keywords
- silk
- super capacitor
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- electrode
- capacitor material
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- 239000000463 material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000003990 capacitor Substances 0.000 title claims abstract description 24
- 239000003610 charcoal Substances 0.000 claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 9
- 230000004913 activation Effects 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000003792 electrolyte Substances 0.000 claims abstract description 5
- 238000005554 pickling Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 14
- 238000003837 high-temperature calcination Methods 0.000 claims description 13
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 239000000428 dust Substances 0.000 claims description 6
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- 239000011149 active material Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000010008 shearing Methods 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000005611 electricity Effects 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 claims description 2
- 239000010419 fine particle Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims 1
- 239000007864 aqueous solution Substances 0.000 claims 1
- 238000010828 elution Methods 0.000 claims 1
- 229910017604 nitric acid Inorganic materials 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 230000001681 protective effect Effects 0.000 abstract description 3
- 241000255789 Bombyx mori Species 0.000 description 7
- 239000003575 carbonaceous material Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical group Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 3
- 238000000840 electrochemical analysis Methods 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method 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
-
- 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
-
- 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
- H01G11/84—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
-
- 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)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The present invention proposes preparation method of super capacitor material and products thereof and application.This method by being pre-processed to silk, high temperature cabonization, pickling, the treatment processes such as activation, silk charcoal is prepared, the silk charcoal of preparation is applied in super capacitor material, tests its chemical property using three-electrode system, in the case where 1mol/L NaOH is electrolyte conditions, prepared silk charcoal has preferable chemical property, and silk of the present invention is from a wealth of sources, low in cost, preparation method is simple and efficient, it is easy to operate, it is environmentally protective, it is easy to be mass produced.
Description
Technical field
The invention belongs to Material Fields, and in particular to the preparation method of a kind of super capacitor material and products thereof and answer
With applied to electrochemical energy storage field.
Background technique
With the development of technology, biomass energy storage is increasingly becoming one of hot topic of the energy.Because with non-renewable energy
Exhaustion, sustainable development is next greatest problem that the entire mankind face in face of existence.And living resources largely may be used
Regeneration, cheap and easy to get and widely distributed, the development of charcoal, moreover it is possible to improve the utilization rate of biological raw material, reduce abandoned biomass
Bring environmental problem.
According to textual criticism, application of the silk in China has more than 5,000 years history, and all the time, working people is to utilize silkworm
Silk manufactures silk thread, braided wires band and simple silk goods.Silk is most light most soft most thin natural fiber in nature, mainly
Because containing a large amount of protein in silk, it can be made in addition in dress material field by various processing methods chemically or physically
It plays outside its good fiber function, may be developed that various new functional materials, widen the new application of silk.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of that present invention to provide a kind of preparation methods for wrapping up IR780@silica nodule.
Another object of the present invention is: providing a kind of package IR780@silica nodule product of above method preparation.
Another object of the present invention is to: a kind of application of the said goods is provided.
The object of the invention pass through following proposal realize: a kind of preparation method of super capacitor material, by silk into
The treatment processes preparation such as row pretreatment, high temperature cabonization, pickling, activation, includes the following steps:
(1) silk that experiment uses is pre-processed: is crushed and cleaned, dried, obtain pre- in drying box after removing particle spot
Treated material
(2) pretreated material is put into tube furnace and carries out high-temperature calcination under an inert atmosphere；
(3) dilute hydrochloric acid is used to wash first in the mixture after high-temperature calcination, then deionized water washing repeatedly, obtains after drying
Silk charcoal；
(4) silk charcoal is activated with dust technology, is obtained for super capacitor material.
Wherein, step (1) pulverising step is conventional magnetic shear means, and silk cocoon shearing is ground into fine particle；It is described
Cleaning step be using deionized water, by the deionized water clean dirt of the particle after shearing.
The inert atmosphere for carrying out high-temperature calcination in step (2) under an inert atmosphere is nitrogen or argon gas.
On the basis of above scheme, the high-temperature calcination is 700-900 DEG C, keeps the temperature 3-6 hours, and heating rate is 1-5 DEG C
Per minute.
The washing of dilute hydrochloric acid described in step (3) is that the hydrochloric acid that the dispersion of calcined powder is placed in 0.1-1mol/L is water-soluble
It is 3-6 hours ultrasonic in liquid.
The activation of dust technology described in step (4) is that the powder dispersion after step (3) drying is placed in the nitre of 0.1-3mol/L
In aqueous acid, impregnate 12-48 hours.
The present invention also provides a kind of super capacitor materials, are prepared according to any of the above-described the method.
The present invention provides a kind of super capacitor material in supercapacitor as the application of working electrode, wherein three
Electrode appraisement system tests its chemical property, is platinum plate electrode, ginseng to electrode in the case where 1mol/L NaOH is electrolyte conditions
It is Ag/AgCl electrode than electrode, working electrode is the electrode of silk charcoal active material accounting 80%.
The invention proposes a kind of preparation method of silk charcoal and its application in supercapacitor, solve existing
There is supercapacitor carbon material preparation process many and diverse, condition is harsh, and environmental pollution is big, the tediously long disadvantage of step, the charcoal system
Preparation Method is easy to operate, and simple process, raw material sources are extensive, low in cost, and easy to operate, environmentally protective, is easy to extensive
Production.
For this purpose, proposing present inventors studied the preparation method that silk prepares biological carbon materials and answering silk charcoal
For in supercapacitor, being compared to other biological charcoal, its chemical property is tested using three-electrode system, in 1mol/L
NaOH is under electrolyte conditions, and prepared silk charcoal has preferable chemical property, and silk of the present invention comes
Source is extensive, low in cost, and preparation method is simple and efficient, easy to operate, environmentally protective, is easy to be mass produced.
Detailed description of the invention
Fig. 1 is 1 SEM of embodiment figure；
Fig. 2 is 1 CV of embodiment figure.
Specific embodiment
The present invention is described in detail by following specific example, but protection scope of the present invention is not only restricted to these
Examples of implementation.
Embodiment 1:
A kind of super capacitor material, is prepared according to the following steps:
10g silk is weighed, silk is pre-processed: being crushed and is cleaned, is dried after removing particle spot in drying box；
Material after drying is put into tube furnace and carries out high-temperature calcination under an inert atmosphere, temperature is 700 DEG C, 6 hours are kept the temperature,
Heating rate is 5 DEG C per minute；
1M dilute hydrochloric acid is used to wash first in the mixture after high-temperature calcination, then deionized water washing repeatedly, obtains after drying
Silk charcoal；
Silkworm excrement charcoal 3M dust technology is activated, material is used as super capacitor material.
Material is prepared into test electrode, electro-chemical test is three-electrode system, and working electrode is that the silkworm excrement after activation is raw
The test electrode of object Carbon Materials preparation, is platinum plate electrode to electrode, reference electrode is saturated calomel electrode.Fast 2mv/s is swept, is electrolysed
Liquid is 1M NaOH.Fig. 1 is SEM figure after silk calcining, and Fig. 2 is to sweep CV under fast 2mv/s to scheme, and electrolyte is 1M NaOH, reference electricity
Extremely Ag/AgCl electrode, is platinum plate electrode to electrode, and working electrode is the electrode of silk charcoal active material accounting 80%, meter
Calculating its capacity is 145F/g.
Embodiment 2:
A kind of super capacitor material, is prepared according to the following steps:
10g silk is weighed, silk is pre-processed: being crushed and is cleaned, is dried after removing particle spot in drying box；
Material after drying is put into tube furnace and carries out high-temperature calcination under an inert atmosphere, temperature is 800 DEG C, 6 hours are kept the temperature,
Heating rate is 3 DEG C per minute；
0.1M dilute hydrochloric acid is used to wash first in the mixture after high-temperature calcination, then deionized water washing repeatedly, obtains after drying
To silk charcoal；
Silkworm excrement charcoal 2M dust technology is activated, material is used as super capacitor material.
Material is prepared into test electrode, electro-chemical test is three-electrode system, and working electrode is that the silkworm excrement after activation is raw
The test electrode of object Carbon Materials preparation, is platinum plate electrode to electrode, reference electrode is saturated calomel electrode.
Embodiment 3:
A kind of super capacitor material, is prepared according to the following steps:
10g silk is weighed, silk is pre-processed: being crushed and is cleaned, is dried after removing particle spot in drying box；
Material after drying is put into tube furnace and carries out high-temperature calcination under an inert atmosphere, temperature is 900 DEG C, 6 hours are kept the temperature,
Heating rate is 1 DEG C per minute；
0.5M dilute hydrochloric acid is used to wash first in the mixture after high-temperature calcination, then deionized water washing repeatedly, obtains after drying
To silk charcoal；
Silkworm excrement charcoal 1M dust technology is activated, material is used as super capacitor material.
Material is prepared into test electrode, electro-chemical test is three-electrode system, and working electrode is that the silkworm excrement after activation is raw
The test electrode of object Carbon Materials preparation, is platinum plate electrode to electrode, reference electrode is saturated calomel electrode.
Claims (8)
1. a kind of preparation method of super capacitor material, which is characterized in that by being pre-processed to silk, high temperature cabonization,
The preparation of the treatment processes such as pickling, activation, includes the following steps:
(1) silk that experiment uses is pre-processed: is crushed and cleaned, dried, obtain pre- in drying box after removing particle spot
Treated material；
(2) pretreated material is put into tube furnace and carries out high-temperature calcination under an inert atmosphere；
(3) dilute hydrochloric acid is used to wash first in the mixture after high-temperature calcination, then deionized water is washed repeatedly, dried, and is obtained
Silk charcoal；
(4) silk charcoal is activated with dust technology, is obtained for super capacitor material.
2. the preparation method of super capacitor material according to claim 1, which is characterized in that in step (1), the crushing
Step are as follows: silk cocoon shearing is ground into fine particle by conventional magnetic shear means；The cleaning step is that will be cut using deionized water
Particle deionized water clean dirt after cutting.
3. the preparation method of super capacitor material according to claim 1, which is characterized in that in indifferent gas in step (2)
The inert atmosphere that high-temperature calcination is carried out under atmosphere is nitrogen or argon gas.
4. according to claim 1 or the preparation method of 3 super capacitor materials, which is characterized in that height described in step (2)
Warm calcining is 700-900 DEG C, keeps the temperature 3-6 hours, and heating rate is 1-5 DEG C per minute.
5. the preparation method of super capacitor material according to claim 1, which is characterized in that dilute salt described in step (3)
Acid elution is that the dispersion of calcined powder is placed in the aqueous hydrochloric acid solution of 0.1-1mol/L, 3-6 hours ultrasonic.
6. the preparation method of super capacitor material according to claim 1, which is characterized in that dilute nitre described in step (4)
Acid activation is that the powder dispersion after step (3) drying is placed in the aqueous solution of nitric acid of 0.1-3mol/L, is impregnated 12-48 hours.
7. a kind of super capacitor material, it is characterised in that -6 any the methods are prepared according to claim 1.
8. a kind of super capacitor material according to claim 7 in supercapacitor as the application of working electrode,
In, three electrode appraisement systems test its chemical property, are platinized platinum electricity to electrode in the case where 1mol/L NaOH is electrolyte conditions
Pole, reference electrode are Ag/AgCl electrode, and working electrode is the electrode of silk charcoal active material accounting 80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811627198.0A CN109671573A (en) | 2018-12-28 | 2018-12-28 | A kind of preparation method of super capacitor material and products thereof and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811627198.0A CN109671573A (en) | 2018-12-28 | 2018-12-28 | A kind of preparation method of super capacitor material and products thereof and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109671573A true CN109671573A (en) | 2019-04-23 |
Family
ID=66147396
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811627198.0A Pending CN109671573A (en) | 2018-12-28 | 2018-12-28 | A kind of preparation method of super capacitor material and products thereof and application |
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| Country | Link |
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| CN (1) | CN109671573A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112964764A (en) * | 2021-02-05 | 2021-06-15 | 深圳市刷新智能电子有限公司 | Electrode for detecting sweat marker and sweat sensor |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007224434A (en) * | 2006-02-21 | 2007-09-06 | Gunma Univ | Carbonized cocoon or silk material and method for producing the same |
| CN104003371A (en) * | 2014-06-11 | 2014-08-27 | 安徽工业大学 | Method for preparing porous carbon material used for super capacitor through using cashmere wool as raw material |
| CN105502383A (en) * | 2015-11-30 | 2016-04-20 | 北京化工大学 | Silkworm cocoon-based hierarchical porous carbon and preparation method thereof |
| CN107215871A (en) * | 2017-06-30 | 2017-09-29 | 海南大学 | A kind of preparation method of activated carbon for super capacitors |
| CN108538630A (en) * | 2017-10-08 | 2018-09-14 | 北京化工大学 | A kind of preparation method of biomass carbon/graphene flexible compound film |
-
2018
- 2018-12-28 CN CN201811627198.0A patent/CN109671573A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007224434A (en) * | 2006-02-21 | 2007-09-06 | Gunma Univ | Carbonized cocoon or silk material and method for producing the same |
| CN104003371A (en) * | 2014-06-11 | 2014-08-27 | 安徽工业大学 | Method for preparing porous carbon material used for super capacitor through using cashmere wool as raw material |
| CN105502383A (en) * | 2015-11-30 | 2016-04-20 | 北京化工大学 | Silkworm cocoon-based hierarchical porous carbon and preparation method thereof |
| CN107215871A (en) * | 2017-06-30 | 2017-09-29 | 海南大学 | A kind of preparation method of activated carbon for super capacitors |
| CN108538630A (en) * | 2017-10-08 | 2018-09-14 | 北京化工大学 | A kind of preparation method of biomass carbon/graphene flexible compound film |
Non-Patent Citations (2)
| Title |
|---|
| JIANHUA HOU等: ""Hierarchical Porous Nitrogen-Doped Carbon Nanosheets Derived from Silk for Ultrahigh-Capacity Battery Anodes and Supercapacitors"", 《ACSNANO》 * |
| 刘玉荣: "《介孔碳材料的很撑及应用》", 30 June 2012 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112964764A (en) * | 2021-02-05 | 2021-06-15 | 深圳市刷新智能电子有限公司 | Electrode for detecting sweat marker and sweat sensor |
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Application publication date: 20190423 |