CN110277249A - A method of high-performance super capacitor negative electrode material is prepared using passion fruit shell - Google Patents
A method of high-performance super capacitor negative electrode material is prepared using passion fruit shell Download PDFInfo
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- CN110277249A CN110277249A CN201910584115.2A CN201910584115A CN110277249A CN 110277249 A CN110277249 A CN 110277249A CN 201910584115 A CN201910584115 A CN 201910584115A CN 110277249 A CN110277249 A CN 110277249A
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- passion fruit
- fruit shell
- super capacitor
- electrode material
- negative electrode
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- 244000288157 Passiflora edulis Species 0.000 title claims abstract description 82
- 235000000370 Passiflora edulis Nutrition 0.000 title claims abstract description 82
- 239000003990 capacitor Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 66
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 25
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 23
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004202 carbamide Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000007772 electrode material Substances 0.000 claims abstract description 15
- 230000008569 process Effects 0.000 claims abstract description 15
- 230000007935 neutral effect Effects 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 239000002699 waste material Substances 0.000 claims abstract description 8
- 230000000717 retained effect Effects 0.000 claims abstract 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000012153 distilled water Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000007833 carbon precursor Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 238000005507 spraying Methods 0.000 claims description 14
- 238000003763 carbonization Methods 0.000 claims description 13
- 239000011149 active material Substances 0.000 claims description 12
- 239000003792 electrolyte Substances 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 11
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000006230 acetylene black Substances 0.000 claims description 9
- 239000010405 anode material Substances 0.000 claims description 9
- 238000002474 experimental method Methods 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- 239000012190 activator Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 229920002678 cellulose Polymers 0.000 claims description 7
- 239000001913 cellulose Substances 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 239000004615 ingredient Substances 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 230000003064 anti-oxidating effect Effects 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 231100000956 nontoxicity Toxicity 0.000 abstract description 3
- 231100001261 hazardous Toxicity 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 21
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 7
- 125000004122 cyclic group Chemical group 0.000 description 6
- 241000208340 Araliaceae Species 0.000 description 5
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 5
- 235000003140 Panax quinquefolius Nutrition 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 235000008434 ginseng Nutrition 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- 238000004146 energy storage Methods 0.000 description 4
- 230000003321 amplification Effects 0.000 description 2
- 230000003026 anti-oxygenic effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 239000002033 PVDF binder Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 235000013311 vegetables Nutrition 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
-
- 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)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of methods for preparing high-performance super capacitor negative electrode material using passion fruit shell, more particularly to new energy environment-friendly materials field, include following steps: step 1: feeding crushes, selection waste type passion fruit shell is raw material, passion fruit shell is rinsed, crush and is screened, passion fruit shell powder is retained.The present invention is mixed by using passion fruit shell powder, potassium hydroxide and the urea of proper ratio, and production process is simple, easily controllable and scale；Multistep carbonizes so that product physical, chemical stability height, can obtain the biological carbon material of high-energy density and power density, the feature of environmental protection is strong；Wherein raw material sources are extensively at low cost, advantageously account for energy shortage problem, reduce electrode material cost, in addition its preferable energy density and the feature that power density, use process nontoxicity are non-hazardous, service life cycle is long, have vast application prospect on neutral aqueous super capacitor field.
Description
Technical field
The present invention relates to new energy environment-friendly materials fields, it is more particularly related to which a kind of utilize passion fruit shell
The method for preparing high-performance super capacitor negative electrode material.
Background technique
With increasingly developed, modern science and technology society need storage and the energy using different scales of science and technology, therefore
Need to design big and small energy resource system, wherein electrical energy storage system is causing the great interest of people in the past few decades.
Supercapacitor is also known as super capacitor or electrochemical double layer capacitor, is that a kind of power density is high, charge/discharge speed is fast, using the longevity
Order long energy storage device.When needing the electrical energy transportation or absorption of high-speed, it can be mended in power storage and collection application
It fills or substituting battery.Compact ultracapacitor can be integrated with microelectronic device, deposits as independent power supply or the efficient energy
Storage unit, as the supplement of battery and energy harvester, so that these equipment be made to be more widely used in many industries.Respectively
Kind Carbon Materials have been studied the material as super capacitor pole with prospects, and biomass carbon material obtains in supercapacitor
To being widely applied.Due to the different form of carbon material, the design of electrode of super capacitor is also not quite similar.Passion fruit is called
Vegetables, feed can be eaten or be done to love fruit, fruit raw.But its shell is not utilized, and can only be abandoned, the present invention utilizes discarded hundred
Fragrant shell is handled by high temperature cabonization, prepares porous activated carbon, therefore have wide development space on energy storage.
Summary of the invention
In order to overcome the drawbacks described above of the prior art, the embodiment of the present invention, which provides, a kind of prepares high property using passion fruit shell
The method of energy super capacitor anode material is carried out by using the passion fruit shell powder, potassium hydroxide and urea of proper ratio
Mixing can be made by three mixing, dehydration, charing steps, and production process is simple, and use is safe, easily controllable and scale
Change, influences each other between experimental procedure small, reduce experimental error；Multistep carbonizes so that product physical, chemical stability height, energy
The biological carbon material of high-energy density and power density is accessed, the feature of environmental protection is strong；Wherein raw material sources are extensively at low cost, are conducive to solve
Certainly energy shortage problem also effectively reduces electrode material cost, in addition its preferable energy density and power density, used
The feature that journey nontoxicity is non-hazardous, service life cycle is long, has vast application on neutral aqueous super capacitor field
Prospect.
To achieve the above object, the invention provides the following technical scheme: it is a kind of super using passion fruit shell preparation high-performance
The method of capacitor anode material, the method for preparing high-performance super capacitor negative electrode material using passion fruit shell include
Following steps:
Step 1: feeding crushes, and selection waste type passion fruit shell is raw material, and passion fruit shell is placed in leakage sieve, is made
During being rinsed with distilled water, need to stir the passion fruit shell inside leakage sieve repeatedly, until passion fruit shell is rinsed well,
It is put into be dried at a certain temperature in baking oven and be completely dried, then move in pulverizer and crushed, then separated with sieve
Biggish particle retains passion fruit shell powder；
Step 2: being mixed,, will using potassium hydroxide and urea as activator using passion fruit shell powder as raw material
It is mixed, distilled water is internally added as solvent, is stirred for uniform, will be obtained under certain temperature environment
Mixture is completely dried, and drying temperature is maintained at 105 DEG C, to obtain carbon precursor；
Step 3: by the carbon precursor after drying, step carbonation is carried out at high temperature, cellulose in passion fruit shell etc. is poly-
It closes object to carbonize to form carbon skeleton, be cleaned with a large amount of distilled water, remove the ingredients such as remaining potassium hydroxide, urea, after vacuum drying,
Obtained product is black solid, i.e., biological carbon material；
Step 4: production electrode, by porous carbon obtained above (active material), acetylene black, Kynoar in mortar
Middle grinding is then added n,N-Dimethylformamide (DMF) solvent and is uniformly mixed and is coated on stainless (steel) wire 1*1cm2, by electrode
Put 80 DEG C of vacuum drying 12h in a vacuum drying oven, obtained electrode material；
Step 5: electrode surface is polished into shiny surface, and carries out spraying operation in electrode surface by polishing spray, wherein
Using oxidation-resistant material as spraying raw material, electrode surface is sprayed uniform.
In a preferred embodiment, the baking oven in the step 1 is dried under the conditions of being maintained at 90 DEG C, does
The dry time is half an hour.
In a preferred embodiment, it is screened, is rejected tiny using the sieve of 200 mesh in the step 1
Graininess shell, and retain subtle shell powder.
In a preferred embodiment, the mixture in the step 3 needs to be placed on inside tube furnace, in argon
Under gas shielded, first step carbonization process: being heat-treated 2 hours in the environment of the mixture after preliminarily dried is placed on 750 DEG C, with
Afterwards carry out second step carbonization process: be heat-treated 1 hour in the environment of mixture is placed on 1150 DEG C, heating rate for 2 DEG C/
Min, cooled to room temperature obtain black product.
In a preferred embodiment, it is needed product before distilled water flushing in the step 3 with 3MHCl
It is cleaned multiple times, serves as removal impurity, be then washed with distilled water to neutral PH=7, the sample after cleaning is at 95 DEG C
Vacuum drying, obtains target product porous carbon.
In a preferred embodiment, it uses stainless (steel) wire as collector in the step 4, is assembled into capacitor
It is tested, the porous carbon materials for loading this experiment preparation are working electrode, and using 3MKCl solution as electrolyte, double salt bridges are
Reference electrode, the excellent big specific capacitance super capacitor anode material of processability.
In a preferred embodiment, the porous carbon (active material) in the step 4, acetylene black, polyvinylidene fluoride
The mass ratio of alkene is 8:1:1.
In a preferred embodiment, the oxidation-resistant material in the step 5 uses aerosil.
Technical effect and advantage of the invention:
1, the present invention is mixed by using passion fruit shell powder, potassium hydroxide and the urea of proper ratio, by mixed
Closing, be dehydrated, carbonizing three steps is that can be made into, and production process is simple, and use is safe, easily controllable and scale, experimental procedure
Between influence each other small, reduce experimental error；Multistep carbonizes so that product physical, chemical stability height, can obtain high energy
The biological carbon material of metric density and power density, the feature of environmental protection are strong；Wherein raw material sources are extensively at low cost, advantageously account for energy shortage
Problem also effectively reduces electrode material cost, in addition its preferable energy density and power density, use process nontoxicity nothing
The long feature of harm, service life cycle, has vast application prospect on neutral aqueous super capacitor field；
2, the present invention is coated with the aerosil of antioxygenic property by electrode material surface after shaping, has
The inoxidizability for improving the electrode material of effect, greatly extends its service life, shortens the replacement frequency of electrode material
Rate.
Detailed description of the invention
Fig. 1 is the SEM image schematic diagram in the present invention under porous carbon materials 2.0k amplification factor.
Fig. 2 is the SEM schematic diagram in the present invention under porous carbon materials 10.0k amplification factor.
Fig. 3 is the different cyclic voltammetric schematic diagrames for sweeping active material under speed in the present invention.
Fig. 4 is the constant current charge-discharge schematic diagram of active material under different current densities in the present invention.
Fig. 5 is the AC impedance schematic diagram of active material in the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention 1-5, technical solution in the embodiment of the present invention carry out it is clear,
It is fully described by, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts it is all its
His embodiment, shall fall within the protection scope of the present invention.
Embodiment 1:
The present invention provides a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell, features
It is, the method for preparing high-performance super capacitor negative electrode material using passion fruit shell includes following steps:
Step 1: feeding crushes, and selection waste type passion fruit shell is raw material, and passion fruit shell is placed in leakage sieve, is made
During being rinsed with distilled water, need to stir the passion fruit shell inside leakage sieve repeatedly, until passion fruit shell is rinsed well,
It is put into be dried at a certain temperature in baking oven and be completely dried, wherein baking oven is dried under the conditions of being maintained at 90 DEG C, drying time
It for half an hour, then moves in pulverizer and is crushed, then screened using the sieve of 200 mesh, reject tiny particle
Shape shell, and retain subtle shell powder；
Step 2: being mixed, using passion fruit shell powder as raw material, using potassium hydroxide and urea as activator,
The mass ratio of middle passion fruit shell powder, potassium hydroxide and urea is 1:1.5:2, is blended together, and distillation is internally added
Water is stirred for uniformly, being completely dried obtained mixture under certain temperature environment, drying temperature is kept as solvent
At 105 DEG C, to obtain carbon precursor；
Step 3: by the carbon precursor after drying, step carbonation is carried out at high temperature, mixture needs to be placed on tube furnace
Inside, under protection of argon gas, first step carbonization process: in the environment of the mixture after preliminarily dried is placed on 750 DEG C at heat
Reason 2 hours then carries out second step carbonization process: being heat-treated 1 hour in the environment of mixture is placed on 1150 DEG C, heating speed
Rate is 2 DEG C/min, and cooled to room temperature obtains black product, and the polymer such as cellulose in passion fruit shell carbonize to form carbon
Product is cleaned multiple times with 3MHCl for skeleton, is served as removal impurity, is then washed with distilled water to neutral PH=7, removes
Ingredients, the samples after cleaning such as remaining potassium hydroxide, urea is gone to be dried in vacuo at 95 DEG C, obtained product is solid for black
Body, i.e., biological carbon material；
Step 4: production electrode, by porous carbon obtained above (active material), acetylene black, the quality of Kynoar
Than being ground in mortar for 8:1:1, n,N-Dimethylformamide (DMF) solvent is then added and is uniformly mixed and is coated on stainless steel
Net 1*1cm2 is assembled into capacitor and is tested using stainless (steel) wire as collector, loads the porous carbon materials of this experiment preparation
For working electrode, using 3MKCl solution as electrolyte, double salt bridges are reference electrode, and electrode is put 80 DEG C in a vacuum drying oven
It is dried in vacuo 12h, is prepared into the big specific capacitance super capacitor anode material haveing excellent performance；
Step 5: electrode surface is polished into shiny surface, and carries out spraying operation in electrode surface by polishing spray, with anti-
Oxidation material is as spraying raw material, and wherein oxidation-resistant material uses aerosil, electrode surface is sprayed uniform；
Step 6: performance test tests electrode material in the method for three electrodes, and wherein electrolyte is 3MKCl, ginseng
It is double salt bridge electrodes than electrode, is platinized platinum to electrode, carries out cyclic voltammetric (CV), AC impedance (EIS), time-measuring electric potential respectively
(GCD) electrochemical property test.
Embodiment 2:
The present invention provides a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell, features
It is, the method for preparing high-performance super capacitor negative electrode material using passion fruit shell includes following steps:
Step 1: feeding crushes, and selection waste type passion fruit shell is raw material, and passion fruit shell is placed in leakage sieve, is made
During being rinsed with distilled water, need to stir the passion fruit shell inside leakage sieve repeatedly, until passion fruit shell is rinsed well,
It is put into be dried at a certain temperature in baking oven and be completely dried, wherein baking oven is dried under the conditions of being maintained at 90 DEG C, drying time
It for half an hour, then moves in pulverizer and is crushed, then screened using the sieve of 200 mesh, reject tiny particle
Shape shell, and retain subtle shell powder；
Step 2: being mixed, using passion fruit shell powder as raw material, using potassium hydroxide and urea as activator,
The mass ratio of middle passion fruit shell powder, potassium hydroxide and urea is 1:2:1, is blended together, distilled water is internally added
As solvent, it is stirred for uniformly, being completely dried obtained mixture under certain temperature environment, drying temperature is maintained at
105 DEG C, to obtain carbon precursor；
Step 3: by the carbon precursor after drying, step carbonation is carried out at high temperature, mixture needs to be placed on tube furnace
Inside, under protection of argon gas, first step carbonization process: in the environment of the mixture after preliminarily dried is placed on 750 DEG C at heat
Reason 2 hours then carries out second step carbonization process: being heat-treated 1 hour in the environment of mixture is placed on 1150 DEG C, heating speed
Rate is 2 DEG C/min, and cooled to room temperature obtains black product, and the polymer such as cellulose in passion fruit shell carbonize to form carbon
Product is cleaned multiple times with 3MHCl for skeleton, is served as removal impurity, is then washed with distilled water to neutral PH=7, removes
Ingredients, the samples after cleaning such as remaining potassium hydroxide, urea is gone to be dried in vacuo at 95 DEG C, obtained product is solid for black
Body, i.e., biological carbon material；
Step 4: production electrode, by porous carbon obtained above (active material), acetylene black, the quality of Kynoar
Than being ground in mortar for 8:1:1, n,N-Dimethylformamide (DMF) solvent is then added and is uniformly mixed and is coated on stainless steel
Net 1*1cm2 is assembled into capacitor and is tested using stainless (steel) wire as collector, loads the porous carbon materials of this experiment preparation
For working electrode, using 3MKCl solution as electrolyte, double salt bridges are reference electrode, and electrode is put 80 DEG C in a vacuum drying oven
It is dried in vacuo 12h, is prepared into the big specific capacitance super capacitor anode material haveing excellent performance；
Step 5: electrode surface is polished into shiny surface, and carries out spraying operation in electrode surface by polishing spray, with anti-
Oxidation material is as spraying raw material, and wherein oxidation-resistant material uses aerosil, electrode surface is sprayed uniform；
Step 6: performance test tests electrode material in the method for three electrodes, and wherein electrolyte is 3MKCl, ginseng
It is double salt bridge electrodes than electrode, is platinized platinum to electrode, carries out cyclic voltammetric (CV), AC impedance (EIS), time-measuring electric potential respectively
(GCD) electrochemical property test.
Embodiment 3:
The present invention provides a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell, features
It is, the method for preparing high-performance super capacitor negative electrode material using passion fruit shell includes following steps:
Step 1: feeding crushes, and selection waste type passion fruit shell is raw material, and passion fruit shell is placed in leakage sieve, is made
During being rinsed with distilled water, need to stir the passion fruit shell inside leakage sieve repeatedly, until passion fruit shell is rinsed well,
It is put into be dried at a certain temperature in baking oven and be completely dried, wherein baking oven is dried under the conditions of being maintained at 90 DEG C, drying time
It for half an hour, then moves in pulverizer and is crushed, then screened using the sieve of 200 mesh, reject tiny particle
Shape shell, and retain subtle shell powder；
Step 2: being mixed, using passion fruit shell powder as raw material, using potassium hydroxide and urea as activator,
The mass ratio of middle passion fruit shell powder, potassium hydroxide and urea is 1:1.25:1.5, is blended together, and is internally added and steams
Distilled water is stirred for uniformly, being completely dried obtained mixture under certain temperature environment, drying temperature is protected as solvent
It holds at 105 DEG C, to obtain carbon precursor；
Step 3: by the carbon precursor after drying, step carbonation is carried out at high temperature, mixture needs to be placed on tube furnace
Inside, under protection of argon gas, first step carbonization process: in the environment of the mixture after preliminarily dried is placed on 750 DEG C at heat
Reason 2 hours then carries out second step carbonization process: being heat-treated 1 hour in the environment of mixture is placed on 1150 DEG C, heating speed
Rate is 2 DEG C/min, and cooled to room temperature obtains black product, and the polymer such as cellulose in passion fruit shell carbonize to form carbon
Product is cleaned multiple times with 3MHCl for skeleton, is served as removal impurity, is then washed with distilled water to neutral PH=7, removes
Ingredients, the samples after cleaning such as remaining potassium hydroxide, urea is gone to be dried in vacuo at 95 DEG C, obtained product is solid for black
Body, i.e., biological carbon material；
Step 4: production electrode, by porous carbon obtained above (active material), acetylene black, the quality of Kynoar
Than being ground in mortar for 8:1:1, n,N-Dimethylformamide (DMF) solvent is then added and is uniformly mixed and is coated on stainless steel
Net 1*1cm2 is assembled into capacitor and is tested using stainless (steel) wire as collector, loads the porous carbon materials of this experiment preparation
For working electrode, using 3MKCl solution as electrolyte, double salt bridges are reference electrode, and electrode is put 80 DEG C in a vacuum drying oven
It is dried in vacuo 12h, is prepared into the big specific capacitance super capacitor anode material haveing excellent performance；
Step 5: electrode surface is polished into shiny surface, and carries out spraying operation in electrode surface by polishing spray, with anti-
Oxidation material is as spraying raw material, and wherein oxidation-resistant material uses aerosil, electrode surface is sprayed uniform；
Step 6: performance test tests electrode material in the method for three electrodes, and wherein electrolyte is 3MKCl, ginseng
It is double salt bridge electrodes than electrode, is platinized platinum to electrode, carries out cyclic voltammetric (CV), AC impedance (EIS), time-measuring electric potential respectively
(GCD) electrochemical property test.
Embodiment 4:
The present invention provides a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell, features
It is, the method for preparing high-performance super capacitor negative electrode material using passion fruit shell includes following steps:
Step 1: feeding crushes, and selection waste type passion fruit shell is raw material, and passion fruit shell is placed in leakage sieve, is made
During being rinsed with distilled water, need to stir the passion fruit shell inside leakage sieve repeatedly, until passion fruit shell is rinsed well,
It is put into be dried at a certain temperature in baking oven and be completely dried, wherein baking oven is dried under the conditions of being maintained at 90 DEG C, drying time
It for half an hour, then moves in pulverizer and is crushed, then screened using the sieve of 200 mesh, reject tiny particle
Shape shell, and retain subtle shell powder；
Step 2: being mixed, using passion fruit shell powder as raw material, using potassium hydroxide and urea as activator,
The mass ratio of middle passion fruit shell powder, potassium hydroxide and urea is 1:1:1, is blended together, distilled water is internally added
As solvent, it is stirred for uniformly, being completely dried obtained mixture under certain temperature environment, drying temperature is maintained at
105 DEG C, to obtain carbon precursor；
Step 3: by the carbon precursor after drying, step carbonation is carried out at high temperature, mixture needs to be placed on tube furnace
Inside, under protection of argon gas, first step carbonization process: in the environment of the mixture after preliminarily dried is placed on 750 DEG C at heat
Reason 2 hours then carries out second step carbonization process: being heat-treated 1 hour in the environment of mixture is placed on 1150 DEG C, heating speed
Rate is 2 DEG C/min, and cooled to room temperature obtains black product, and the polymer such as cellulose in passion fruit shell carbonize to form carbon
Product is cleaned multiple times with 3MHCl for skeleton, is served as removal impurity, is then washed with distilled water to neutral PH=7, removes
Ingredients, the samples after cleaning such as remaining potassium hydroxide, urea is gone to be dried in vacuo at 95 DEG C, obtained product is solid for black
Body, i.e., biological carbon material；
Step 4: production electrode, by porous carbon obtained above (active material), acetylene black, the quality of Kynoar
Than being ground in mortar for 8:1:1, n,N-Dimethylformamide (DMF) solvent is then added and is uniformly mixed and is coated on stainless steel
Net 1*1cm2 is assembled into capacitor and is tested using stainless (steel) wire as collector, loads the porous carbon materials of this experiment preparation
For working electrode, using 3MKCl solution as electrolyte, double salt bridges are reference electrode, and electrode is put 80 DEG C in a vacuum drying oven
It is dried in vacuo 12h, is prepared into the big specific capacitance super capacitor anode material haveing excellent performance；
Step 5: electrode surface is polished into shiny surface, and carries out spraying operation in electrode surface by polishing spray, with anti-
Oxidation material is as spraying raw material, and wherein oxidation-resistant material uses aerosil, electrode surface is sprayed uniform；
Step 6: performance test tests electrode material in the method for three electrodes, and wherein electrolyte is 3MKCl, ginseng
It is double salt bridge electrodes than electrode, is platinized platinum to electrode, carries out cyclic voltammetric (CV), AC impedance (EIS), time-measuring electric potential respectively
(GCD) electrochemical property test.
Embodiment 5:
The present invention provides a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell, features
It is, the method for preparing high-performance super capacitor negative electrode material using passion fruit shell includes following steps:
Step 1: feeding crushes, and selection waste type passion fruit shell is raw material, and passion fruit shell is placed in leakage sieve, is made
During being rinsed with distilled water, need to stir the passion fruit shell inside leakage sieve repeatedly, until passion fruit shell is rinsed well,
It is put into be dried at a certain temperature in baking oven and be completely dried, wherein baking oven is dried under the conditions of being maintained at 90 DEG C, drying time
It for half an hour, then moves in pulverizer and is crushed, then screened using the sieve of 200 mesh, reject tiny particle
Shape shell, and retain subtle shell powder；
Step 2: being mixed, using passion fruit shell powder as raw material, using potassium hydroxide and urea as activator,
The mass ratio of middle passion fruit shell powder, potassium hydroxide and urea is 1:2:3, is blended together, distilled water is internally added
As solvent, it is stirred for uniformly, being completely dried obtained mixture under certain temperature environment, drying temperature is maintained at
105 DEG C, to obtain carbon precursor；
Step 3: by the carbon precursor after drying, step carbonation is carried out at high temperature, mixture needs to be placed on tube furnace
Inside, under protection of argon gas, first step carbonization process: in the environment of the mixture after preliminarily dried is placed on 750 DEG C at heat
Reason 2 hours then carries out second step carbonization process: being heat-treated 1 hour in the environment of mixture is placed on 1150 DEG C, heating speed
Rate is 2 DEG C/min, and cooled to room temperature obtains black product, and the polymer such as cellulose in passion fruit shell carbonize to form carbon
Product is cleaned multiple times with 3MHCl for skeleton, is served as removal impurity, is then washed with distilled water to neutral PH=7, removes
Ingredients, the samples after cleaning such as remaining potassium hydroxide, urea is gone to be dried in vacuo at 95 DEG C, obtained product is solid for black
Body, i.e., biological carbon material；
Step 4: production electrode, by porous carbon obtained above (active material), acetylene black, the quality of Kynoar
Than being ground in mortar for 8:1:1, n,N-Dimethylformamide (DMF) solvent is then added and is uniformly mixed and is coated on stainless steel
Net 1*1cm2 is assembled into capacitor and is tested using stainless (steel) wire as collector, loads the porous carbon materials of this experiment preparation
For working electrode, using 3MKCl solution as electrolyte, double salt bridges are reference electrode, and electrode is put 80 DEG C in a vacuum drying oven
It is dried in vacuo 12h, is prepared into the big specific capacitance super capacitor anode material haveing excellent performance；
Step 5: electrode surface is polished into shiny surface, and carries out spraying operation in electrode surface by polishing spray, with anti-
Oxidation material is as spraying raw material, and wherein oxidation-resistant material uses aerosil, electrode surface is sprayed uniform；
Step 6: performance test tests electrode material in the method for three electrodes, and wherein electrolyte is 3MKCl, ginseng
It is double salt bridge electrodes than electrode, is platinized platinum to electrode, carries out cyclic voltammetric (CV), AC impedance (EIS), time-measuring electric potential respectively
(GCD) electrochemical property test.
It takes electrode material obtained by above-described embodiment 1-5 to be tested respectively, takes five groups altogether, every 30 are one group, point
The electrode material prepared in five embodiments is tried out respectively for five groups obtain following data after 3 months:
As seen from the above table, raw material mixing ratio is moderate in embodiment 5, and compressive property is higher, physics itself, chemical stability
It is effectively improved, the biological carbon material of high-energy density and power density can be obtained, in addition antioxygenic property also obtains
Great promotion effectively extends its service life, and the feature of environmental protection is strong, has on neutral aqueous super capacitor field wide
Big application prospect.
Last: the foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, all in the present invention
Spirit and principle within, any modification, equivalent replacement, improvement and so on, should be included in protection scope of the present invention it
It is interior.
Claims (8)
1. a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell, which is characterized in that the utilization
The method that passion fruit shell prepares high-performance super capacitor negative electrode material includes following steps:
Step 1: feeding crushes, and selection waste type passion fruit shell is raw material, and passion fruit shell is placed in leakage sieve, steaming is used
During distilled water is rinsed, needs to stir the passion fruit shell inside leakage sieve repeatedly and be put into until passion fruit shell is rinsed well
It is dried to and is completely dried at a certain temperature in baking oven, then move in pulverizer and crushed, then separated with sieve larger
Particle, retain passion fruit shell powder；
Step 2: it is mixed, using passion fruit shell powder as raw material, using potassium hydroxide and urea as activator, is mixed
It is combined, distilled water is internally added as solvent, be stirred for the uniformly mixing that will be obtained under certain temperature environment
Object is completely dried, and drying temperature is maintained at 105 DEG C, to obtain carbon precursor；
Step 3: by the carbon precursor after drying, step carbonation, the polymer such as cellulose in passion fruit shell are carried out at high temperature
Charing forms carbon skeleton, is cleaned with a large amount of distilled water, removes the ingredients such as remaining potassium hydroxide, urea, after vacuum drying, obtains
Product be black solid, i.e., biological carbon material；
Step 4: production electrode grinds porous carbon obtained above (active material), acetylene black, Kynoar in mortar
Mill is then added n,N-Dimethylformamide (DMF) solvent and is uniformly mixed and is coated on stainless (steel) wire 1*1cm2, electrode is put in
80 DEG C of vacuum drying 12h, obtained electrode material in vacuum oven；
Step 5: electrode surface is polished into shiny surface, and carries out spraying operation in electrode surface by polishing spray, wherein with anti-
Oxidation material sprays electrode surface uniform as spraying raw material.
2. a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell according to claim 1,
It is characterized by: the baking oven in the step 1 is dried under the conditions of being maintained at 90 DEG C, drying time is half an hour.
3. a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell according to claim 1,
It is characterized by: being screened in the step 1 using the sieve of 200 mesh, tiny graininess shell is rejected, and is retained thin
Micro- shell powder.
4. a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell according to claim 1,
It is characterized by: the mixture in the step 3 needs to be placed on inside tube furnace, under protection of argon gas, the first step was carbonized
Journey: being heat-treated 2 hours in the environment of the mixture after preliminarily dried is placed on 750 DEG C, then carries out second step carbonization process:
It is heat-treated 1 hour in the environment of mixture is placed on 1150 DEG C, heating rate is 2 DEG C/min, and cooled to room temperature obtains
Black product.
5. a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell according to claim 1,
It is characterized by: needing that product is cleaned multiple times with 3MHCl before distilled water flushing in the step 3, serve as
Except impurity, neutral PH=7 are then washed with distilled water to, the sample after cleaning is dried in vacuo at 95 DEG C, obtains target product
Porous carbon.
6. a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell according to claim 1,
It is characterized by: being assembled into capacitor as collector using stainless (steel) wire in the step 4 and being tested, this experiment system is loaded
Standby porous carbon materials are working electrode, and using 3MKCl solution as electrolyte, double salt bridges are reference electrode, and processability is excellent
Big specific capacitance super capacitor anode material.
7. a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell according to claim 1,
It is characterized by: the mass ratio of porous carbon (active material), acetylene black, Kynoar in the step 4 is 8:1:1.
8. a kind of method for preparing high-performance super capacitor negative electrode material using passion fruit shell according to claim 1,
It is characterized by: the oxidation-resistant material in the step 5 uses aerosil.
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| CN110808179A (en) * | 2019-10-28 | 2020-02-18 | 桂林电子科技大学 | Nitrogen-oxygen co-doped biomass hard carbon material and preparation method and application thereof |
| CN111675217A (en) * | 2020-06-22 | 2020-09-18 | 桂林理工大学 | Supercapacitor electrode material based on peanut bran and preparation method and application thereof |
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| CN107311172A (en) * | 2017-07-18 | 2017-11-03 | 桂林电子科技大学 | A kind of passion fruit shell base porous carbon materials and its preparation method and application |
| CN107785175A (en) * | 2017-10-03 | 2018-03-09 | 长沙仲善新能源科技有限公司 | A kind of solar energy graphene battery |
| CN108550853A (en) * | 2018-05-08 | 2018-09-18 | 姜雪 | A kind of graphene battery positive electrode and preparation method thereof that specific capacity is high |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107311172A (en) * | 2017-07-18 | 2017-11-03 | 桂林电子科技大学 | A kind of passion fruit shell base porous carbon materials and its preparation method and application |
| CN107785175A (en) * | 2017-10-03 | 2018-03-09 | 长沙仲善新能源科技有限公司 | A kind of solar energy graphene battery |
| CN108550853A (en) * | 2018-05-08 | 2018-09-18 | 姜雪 | A kind of graphene battery positive electrode and preparation method thereof that specific capacity is high |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110808179A (en) * | 2019-10-28 | 2020-02-18 | 桂林电子科技大学 | Nitrogen-oxygen co-doped biomass hard carbon material and preparation method and application thereof |
| CN110808179B (en) * | 2019-10-28 | 2022-01-18 | 桂林电子科技大学 | Nitrogen-oxygen co-doped biomass hard carbon material and preparation method and application thereof |
| CN111675217A (en) * | 2020-06-22 | 2020-09-18 | 桂林理工大学 | Supercapacitor electrode material based on peanut bran and preparation method and application thereof |
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