CN110379643A - A kind of preparation method and applications of water hyacinth biomass carbon - Google Patents
A kind of preparation method and applications of water hyacinth biomass carbon Download PDFInfo
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- CN110379643A CN110379643A CN201910675233.4A CN201910675233A CN110379643A CN 110379643 A CN110379643 A CN 110379643A CN 201910675233 A CN201910675233 A CN 201910675233A CN 110379643 A CN110379643 A CN 110379643A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- 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
Abstract
The present invention relates to a kind of water hyacinth applied technical fields, and in particular to a kind of preparation method and applications of water hyacinth biomass carbon；The preparation method step is simple, and using nontoxic NaCl and KCl salt-mixture, a step carbonization-activation can directly prepare charcoal in air atmosphere, and there are carbonization structure abundant and oxygen-containing functional groups for biomass carbon obtained, have good chemical property；It can be with some water hyacinths of recycling treatment, more comprehensively efficiently to be laid the foundation using water hyacinth.
Description
Technical field:
The invention belongs to water hyacinth applied technical fields, and in particular to a kind of preparation method of water hyacinth biomass carbon and its
Using.
Background technique:
Water hyacinth (water hyacinth), originates in Brazil, is perennial floatability herbaceous plant, and resistance to fertility resists
Characteristic of disease is all very strong, is one of to grow in the world, breed most fast water plant；It introduces after China due at home without natural enemy,
Rapidly, after especially reforming and opening up to the outside world, China's rapid economic development, water eutrophication problem is highlighted, and causes water hyacinth crazy for growth
Long, the water hyacinth of overgrowing not only blocks navigation channel, influences shipping and excretion, and limits the flowing of water body, mentions for mosquitos and flies, germ
Breeding ground has been supplied, serious ecological environment problem is brought.And the improvement of water hyacinth is a difficult task, in addition to high
Salvage expenses, the water hyacinth for how handling enormous amount are also a very troublesome problem, and are handled water hyacinth at present and are generally used
It directly fills, but this needs a large amount of soil, and the water hyacinth after landfill can also give out foul smell, worse, because
It has adsorbed the water pollutants such as heavy metal, and landfill is also easy to cause underground water pollution, causes tremendous influence to water environment.
But from the point of view of another angle, the water hyacinth of substantial amounts contains huge biomass resource, if can be by water
Cucurbit resource utilization, so that it may turn waste into wealth, solve the problems, such as water hyacinth；In view of containing a large amount of high-quality porous fibres in water hyacinth
Dimension, can be made the activated carbon of function admirable, realize that hyacinth resource utilization provides new approach to be extensive.Biomass carbon material
Because raw material is easy to get and renewable, adjustable obtain porous structure and be widely used the super capacitor in electrochemical energy storage
Device, but the porous carbon majority of biomass synthesis at present is in inert gas (such as N2And Ar) under carry out, this needs a large amount of
Resource consumption and stringent technology and equipment require higher to material requirements, and it is larger to promote difficulty, to hinder water
The commodity production of cucurbit biomass carbon.
Summary of the invention:
For biomass carbon is prepared at present, there are operating process complexity, preparation process to generate harmful substance, needs consumption big
Measure the defect and problem of resource, the present invention provide it is a kind of it is nontoxic, utilize simple step carbonization-activation and salt to melt technology system
The method of standby water hyacinth biomass carbon.
The present invention solves scheme used by its technical problem: a kind of preparation method of water hyacinth biomass carbon, including
Following steps:
S1, pretreatment: mature living body water hyacinth is chosen, removal jaundice, withered blade are multiple with clean tap water
It rinses, washes away the impurity and sludge on water hyacinth surface；
S2, drying: air-dried surface moisture after washed water hyacinth is cleaned 3-5 times with deionized water is put into baking oven, in
4h is dried under the conditions of 60-100 DEG C, is then crushed with pulverizer, 60 mesh aperture sieves are crossed, and pack is stand-by；
S3, charing: smashed water hyacinth sample is put into crucible, and be completely covered on water hyacinth sample KCl and
NaCl covers crucible lid and is put into Muffle furnace, is warming up to 800 DEG C step by step and keeps 3-4h；
S4, it is naturally cooling to room temperature to Muffle furnace, crucible is taken out, by the water hyacinth sample after charing in 1MHCl solution
2-3h is impregnated, then with the multiple washed product of deionized water and filter until the aqueous solution pH filtered is 7, it will filter after suction filtration
Sample is separated with filter membrane after dry in 120 DEG C of vacuum drying 6h, water hyacinth biomass carbon can be obtained, to water by film and sample
Cucurbit biomass carbon sample is weighed, and is saved backup.
A kind of preparation method of above-mentioned water hyacinth biomass carbon, KCl the and NaCl ratio are 1:1.
A kind of preparation method of above-mentioned water hyacinth biomass carbon, the water hyacinth sample and KCl and NaCl salt-mixture
Ratio is 1:5.
The coverage mode of a kind of preparation method of above-mentioned water hyacinth biomass carbon, the KCl and NaCl are first by the two
It is uniformly mixed, then is covered on water hyacinth sample.
A kind of preparation method of above-mentioned water hyacinth biomass carbon, dry temperature is 80 DEG C in the step S2.
A kind of preparation method of above-mentioned water hyacinth biomass carbon, chosen material is mature water hyacinth in the step S1
Blade position.
A kind of preparation method of above-mentioned water hyacinth biomass carbon, the rate of the heating are 10 DEG C/min.
The present invention also provides a kind of application of water hyacinth biomass carbon, which are mainly applied to preparing electrode of super capacitor,
The following steps are included:
A, the steel wire of 500 mesh is cut into the strip of 12cm × 1.5cm, be cleaned by ultrasonic 3h with 6M NaOH and is impregnated
12h cleans 30min with EtOH Sonicate with after ultrapure water, is placed in baking oven in 60 DEG C of drying 3h, trims flash and remembers subscript
Number, weighing record, sealing storage is for use；
B, the adhesive of the water hyacinth biomass samples of 80wt%, the conductive agent of 15wt% and 5wt% is taken to mix and in second
It is ground uniformly in alcohol, ground sample is uniformly coated on to one end of ready steel wire, is in 60 DEG C of vacuum drying 3h
Supercapacitor working electrode is made.
A kind of application of above-mentioned water hyacinth biomass carbon, described adhesive is Kynoar.
Beneficial effects of the present invention:
1, the present invention prepares biomass carbon using water hyacinth as raw material, is the recycling of solid waste resource, is water calabash
The processing of reed provides approach, more comprehensively efficiently to be laid the foundation using water hyacinth；
2, activation process is adjusted as reaction medium by using KCl and NaCl salt-mixture and directly prepare charcoal, be not required to
Inert gas is consumed, is economized on resources, and KCl and NaCl are nontoxic, a step can be prepared by biomass carbon, to technology, set
Standby of less demanding, step is simple, convenient for promoting；
3, characterization result shows charcoal in irregular multi-layer sheet structure, and the multi-layer sheet structure of WHBC-L is most thin, and accumulation is blocky
Structure is minimum, this is consistent with the specific surface area maximum of WHBC-L in BET result, at the same pore analysis show in three samples with
Based on micropore, there are a small amount of mesoporous, and the presence of carbonization structure and oxygen-containing functional group abundant are all conducive to mention in sample
The chemical property of high sample；
4, WHBC-L shows best chemical property in electro-chemical test, the specific capacitance when current density is 1A/g
122F/g is reached, capacity retention is 67.2% when current density is 10A/g；Symmetric double electricity grade electricity is assembled into WHBC-L
Specific capacitance when container under 0.5A/g current density is 63F/g, has further calculated the energy density and power of symmetric capacitor
Density, energy density are up to 4.375Wh/kg, and power density is 0.035W/kg at this time.
Detailed description of the invention:
Fig. 1 is thermogravimetric analysis figure of the water hyacinth in pyrolytic process；
Fig. 2 is the nitrogen Adsorption and desorption isotherms of WHBC-R, WHBC-S, WHBC-L；
Fig. 3 is the pore size distribution curve of water hyacinth root (WHBC-R)；
Fig. 4 is the pore size distribution curve of water hyacinth stem (WHBC-S)；
Fig. 5 is the pore size distribution curve of water hyacinth blade biomass carbon (WHBC-L)；
Fig. 6 is the scanning electron microscope (SEM) photograph (SEM) of WHBC-R, WHBC-S, WHBC-L under different multiplying；
Fig. 7 is the XRD spectrum of WHBC-R, WHBC-S, WHBC-L；
Fig. 8 is that the electrode of three kinds of water hyacinth biomass carbons preparation sweeps CV curve and GCD curve under speed in 100m V/S；
Fig. 9 is that three kinds of samples carry out the different CV tests swept under speed and the GCD test result under different current densities；
Figure 10 is the EIS curve of WHBC-R, WHBC-S, WHBC-L；
Figure 11 is GCD curve of the WHBC-L symmetric double electricity grade under different current densities.
Specific embodiment:
Present invention will be further explained below with reference to the attached drawings and examples, maturation that this experiment uses, living body water hyacinth are same
Meaning purchase is in Shenzhen water plant farm.
Embodiment 1: the preparation method of the water hyacinth biomass carbon of the present embodiment, comprising the following steps:
S1, pretreatment: the root (Root) of mature living body water hyacinth is chosen, is repeatedly rinsed, is washed with clean tap water
Remove the impurity and sludge of water hyacinth root；
S2, drying: the water hyacinth root samples pre-processed are cleaned 3-5 times with deionized water, are air-dried surface moisture, are put
Enter in baking oven, 4h is dried under the conditions of 80 DEG C, is then crushed with pulverizer, cross 60 mesh aperture sieves, pack is stand-by；
S3, charing: the water hyacinth root samples 3g after weighing drying and crushing are put into cylindrical corundum aluminium crucible, in sample
The top of product is covered each by the uniformly mixed KCl and NaCl (1:1) salt-mixture of 15g, covers crucible lid and is put into Muffle furnace, presses
800 DEG C are warming up to according to the rate of 10 DEG C/min, and keeps 3h at 800 DEG C；
S4, after Muffle furnace is naturally cooling to room temperature, take out crucible, distinguish washed product 5 with deionized water and 1MHCl
It is secondary, sample is separated with filter membrane after dry, be can be obtained with water calabash in 120 DEG C of vacuum drying 6h by filter membrane and sample after suction filtration
Biomass carbon sample is weighed, is saved backup by the biomass carbon that reed root is prepared.
Embodiment 2: the preparation method of the water hyacinth biomass carbon of the present embodiment, comprising the following steps:
S1, pretreatment: the stem (Stalk) of mature living body water hyacinth is chosen, is repeatedly rinsed, is washed with clean tap water
Remove the impurity and sludge of water hyacinth root；
S2, drying: the water hyacinth stem sample pre-processed is cleaned 3-5 times with deionized water, is air-dried surface moisture, is put
Enter in baking oven, 4h is dried under the conditions of 80 DEG C, is then crushed with pulverizer, cross 60 mesh aperture sieves, pack is stand-by；
S3, charing: the water hyacinth stem sample 3g after weighing drying and crushing are put into cylindrical corundum aluminium crucible, in sample
The top of product is covered each by the uniformly mixed KCl and NaCl (1:1) salt-mixture of 15g, covers crucible lid and is put into Muffle furnace, presses
800 DEG C are warming up to according to the rate of 10 DEG C/min, and keeps 3h at 800 DEG C；
S4, after Muffle furnace is naturally cooling to room temperature, take out crucible, distinguish washed product 5 with deionized water and 1MHCl
It is secondary, sample is separated with filter membrane after dry, be can be obtained with water calabash in 120 DEG C of vacuum drying 6h by filter membrane and sample after suction filtration
Biomass carbon sample is weighed, is saved backup by the biomass carbon that reed stem is prepared.
Embodiment 3: the preparation method of the water hyacinth biomass carbon of the present embodiment, comprising the following steps:
S1, pretreatment: choosing the blade (Leaf) of mature living body water hyacinth, the withered blade of removal jaundice, with clean
Tap water repeatedly rinse, wash away the impurity and sludge of water hyacinth root；
S2, drying: the water hyacinth leaf sample pre-processed is cleaned 3-5 times with deionized water, is air-dried surface moisture, is put
Enter in baking oven, 4h is dried under the conditions of 80 DEG C, is then crushed with pulverizer, cross 60 mesh aperture sieves, pack is stand-by；
S3, charing: the water hyacinth leaf sample 3g after weighing drying and crushing are put into cylindrical corundum aluminium crucible, in sample
The top of product is covered each by the uniformly mixed KCl and NaCl (1:1) salt-mixture of 15g, covers crucible lid and is put into Muffle furnace, presses
800 DEG C are warming up to according to the rate of 10 DEG C/min, and keeps 3h at 800 DEG C；
S4, after Muffle furnace is naturally cooling to room temperature, take out crucible, distinguish washed product 5 with deionized water and 1MHCl
It is secondary, sample is separated with filter membrane after dry, be can be obtained with water calabash in 120 DEG C of vacuum drying 6h by filter membrane and sample after suction filtration
Biomass carbon sample is weighed, is saved backup by the biomass carbon that reed blade is prepared.
Embodiment 4: performance test
4.1 thermogravimetric analysis (TG)
Using thermogravimetric analyzer, 800 DEG C are raised to from room temperature in air atmosphere, with the heating rate of 10 DEG C/min, analysis
With the variation of the raising sample quality of temperature and the chemical property of component；Meanwhile water hyacinth is recorded using Differential Scanning Calorimetry
Pyrogram (DSC), as a result as shown in Figure 1, in DSC figure absorb heat effectiveness protrusion peak value characterization, exothermic effect reversed peak
Characterization.
It can be seen from the TG test result and water hyacinth DSC result of Fig. 1 the fusing point higher (685 DEG C) of solid salt to
Up to completely cutting off contact of the presoma with air before fusing point in the form of sealed solid agent, the weight loss of this stage presoma compared with
It is few；Solid salt starts to be diffused into initial carbonized product after melting, and the fused salt a part for being covered on above stays in top and plays liquid
The effect of body sealing；Holding stage is due to foring a large amount of micropore and mesoporous on the corrasion Carbon Materials of liquid salt；Finally
In temperature-fall period, as the more salinities of the extension of time evaporate, more oxygen are brought to infiltrate into system, and then generate more
More micropores；Salinity can play a protective role in water hyacinth biomass combustion, this is because when temperature reaches salinity fusing point
Later, salinity starts to melt, and the salt of molten is diffused into carbonizing production with liquid phase state, is prevented in the form of fluid sealant
Product char burning；When temperature is stablized at 800 DEG C, the salt of molten state acts not only as the effect of fluid sealant, and salt ion may be used also
To etch carbon structure, micropore and central hole structure are formed；In heat preservation and temperature-fall period later, with the extension of time, more
Salinity evaporation, bring more oxygen to infiltrate into system, and then generate more micropores.
4.2 specific surface areas and pore analysis (BET)
By water hyacinth root made from embodiment 1, embodiment 2 and embodiment 3, stem, leaf biomass carbon sample at 150 DEG C
Vacuum drying 8h is pre-processed, and then the biomass carbon by water hyacinth root, stem, leaf preparation measures under the conditions of 77K to liquid nitrogen
Adsorption desorption curve, is as a result shown in Fig. 2；By the data of adsorption curve when relative pressure (P/P0) is between 0.1-0.35, pass through
Brunauer-Emmett-Teller (BET) equation calculation water hyacinth root biomass carbon (WHBC-R), water hyacinth stem biomass carbon
(WHBC-S), the specific surface area of leaves of hyacinth biomass carbon (WHBC-L), and it is flat using non-localized Density Functional Theory (NLDFT)
Weigh model calculated hole diameters.
From figure 2 it can be seen that three kinds of water hyacinth root, stem, leaf biomass carbon Adsorption and desorption isotherms show the absorption of IV type
Feature, the type adsorption isotherm belong to the feature adsorption curve of mesopore material；Three sample discoveries are compared, WHBC-L shows
Maximum nitrogen adsorption capacity, this shows that WHBC-L has the pore structure of large specific surface area, calculates the ratio of three samples
Surface area is respectively 375.45cm3/g、426.95cm3/ g and 582.81cm3/ g, it is consistent with the result showed in figure, it was demonstrated that
WHBC-L has the pore structure of large specific surface area；From Fig. 2 it can also be seen that in the range of relative pressure is less than 0.1,
Three samples show different degrees of adsorbance, show the presence of micropore in sample, while the WHBC-L of maximal absorptive capacity
Micropore is most abundant；When relative pressure is between 0.4-0.9, apparent hysteresis curve is showed, shows the presence of sample intermediary hole,
So the test result shows that there are micropores and mesoporous classification aperture in test sample.
The pore size distribution curve of three kinds of samples is calculated using NLDFT theoretical model, and is normalized, and as a result sees figure
3-5, the results showed that, chief component is micropore in sample aperture, and micropore accounts for about 78%, the WHBC-S in total aperture in WHBC-R
Middle micropore accounts for about micropore in 82%, the WHBC-L in total aperture and accounts for about the 94% of total aperture.
4.3 scanning electron microscope analysis
It is scanned using appearance of the Flied emission Scanning Electron microscope to WHBC-R, WHBC-S, WHBC-L, to characterize sample
The form and microscopic appearance of product, scanning multiple are 1000-20000 times, as a result see Fig. 6.
As seen from Figure 6, it can be observed how that water hyacinth sample shows irregular lamellar structure under low range,
These synusia are irregular to be packed together, and compares the water hyacinth sample of different parts, the sheet accumulation of root (WHBC-R) compared with
Intensively, or even biggish block structure is formed, this will affect the specific surface area of Carbon Materials, the laminated structure shape of stem (WHBC-S)
Shape is less than root, and more small pieces or fritter is distributed around big plate shape, leaf portion (WHBC-L) it is obvious than root and
The laminated structure area of stem is small, and the block structure of random accumulation is also smaller, facilitates the specific surface area for increasing sample；To sample
It is observed after product partial enlargement, the laminated structure thickness of root (WHBC-R) is larger, surface relative smooth；Stem (WHBC-S) sample
Thickness is less than root, and surface is rougher；The laminated structure of leaf portion (WHBC-L) is most thin, and big schistose surface accumulates a large amount of small pieces
Shape structure, and have the appearance of roundlet column structure, two-dimensional sheet structure can shorten the transmission range of ion, to be conducive to electricity
Solve the diffusion of liquid intermediate ion.
4.4 X-ray diffractions (XRD)
WHBC-R, WHBC-S, WHBC-L after pickling is used into the inorganic mineral ash in X-ray diffraction analysis charcoal
Point.Range is 0.5 ° of step-length from 10 ° to 90 °, and sweep speed is 0.1 second/step.
As seen from Figure 7, sample WHBC-L has apparent diffraction peak structure in 23.6 ° and 44 ° of two positions, the two
Diffraction maximum respectively corresponds (002) crystal face and (100) crystal face of graphite, and the diffraction maximum of WHBC-R and WHBC-S (100) crystal face is smaller,
Can only obviously observe (002) crystal face, the two crystal faces there are the degree of graphitization of representative sample, illustrate in three samples
In, the degree of graphitization highest of WHBC-L, this is conducive to improve electron transmission efficiency, to improve the electric conductivity of material.
Embodiment 5: the present embodiment provides a kind of applications of water hyacinth biomass carbon, are mainly used in preparation supercapacitor
Electrode.
5.1 preparation method
A, the steel wire of 500 mesh is cut into the strip of 12cm × 1.5cm, be cleaned by ultrasonic 3h with 6M NaOH and is impregnated
12h cleans 30min with EtOH Sonicate with after ultrapure water, is placed in baking oven in 60 DEG C of drying 3h, trims flash and remembers subscript
Number, weighing record, sealing is deposited stand-by；
B, fetch water cucurbit root, stem, each 80wt% of leaf biomass carbon sample, then respectively with the conductive agent of 15wt% and
The Kynoar of 5wt% mixed grinding in ethanol, is uniformly coated on ready steel wire for ground sample respectively
One end, in 60 DEG C of vacuum drying 3h, sample quality is 2mg to get to three kinds of water hyacinth biomass carbons in final each electrode
Manufactured supercapacitor working electrode.
The test of 5.2 electrode performances
In order to make the electrode material of 5.1 preparations steady operation in test, need to prepare before measuring chemical property
Good working electrode to be measured impregnates a few hours in the electrolytic solution, and electrolyte used in this experiment is 1M H2SO4 solution.
In order to explore prepared water hyacinth charcoal chemical property, compare different parts water hyacinth charcoal chemical property
Between difference.The working electrode of preparation tests WHBC-R, WHBC-S and WHBC-L in 100m under three-electrode system first
V/S sweeps the corresponding GCD curve of the CV curve under speed, sees Fig. 8；Wherein cyclic voltammetry (CV) is tested, and mainly measures work
The electrochemical reaction activity of active material and the invertibity of reaction, CV test voltage range test difference in 0-1V in electrode
Scanning result under sweep speed；Constant current charge-discharge (GCD), can test the charge and discharge of working electrode under different current densities
Electric situation, to calculate the specific capacitance of material, power density and energy density.
CV curve shows similar rectangular shape it can be seen from (a) figure in Fig. 8, by comparison it can be found that
WHBC-L has maximum scan area, this illustrates its capacitive character highest；(b) figure is corresponding GCD curve, measures current density
It is 1A/g, GCD curve shows asymmetric triangle in figure, and WHBC-L also shows that the longest charge and discharge time.
The CV test and not that differences sweep under speed (sweeping speed is respectively 100,80,50,20 and 10mV/S) is carried out to three kinds of samples
With the GCD test of (current density is respectively 1,2,5 and 10A/g) under current density, test result is shown in Fig. 9.
By Fig. 9 it can be found that different sweep the shape that the CV figure line under speed all shows class rectangle, under different current densities
GCD figure presents asymmetric triangular shaped.Current density increases the reduction of charge and discharge time, and WHBC-L is in 1A/gGCD curve sample
WHBC-L charge and discharge total time under the current density of 1A/g is 250s.
5.3 electrochemical analysis
Soaked electrode to be measured in the electrolytic solution will be shifted to an earlier date, its chemical property and ginseng are tested by electrochemical workstation
Number tests the chemical property of carbon material electrode under three-electrode system and two-electrode system respectively；In three-electrode system, choosing
Take Ag/AgCl electrode as reference electrode, platinized platinum is, to electrode, the electrode for being coated with the water hyacinth Carbon Materials of preparation is work electricity
Pole.
Symmetrical twin electrodes system can measure the energy storage situation of material.
The calculation method of the capacitor of electrode to be measured is as follows in three-electrode system:
The calculation method of capacitor is in two-electrode system:
Wherein formula (1), I (unit: A) refers to discharge current in formula (2)；Δ t (unit: s) refers to discharge time；m
(unit: g) refers to the active material i.e. quality of sample in electrode to be measured；Δ V (unit: v) is voltage range.
Calculate the specific capacitance under different current densities using formula (1), formula (2), current density more high specific capacitance more
Small, WHBC-L specific capacitance under 1A/g current density is 122F/g, and the specific capacitance of 113F/g is still maintained under 2A/g current density,
Capacity retention is 92.6%.When current density is increased to 10A/g, specific capacitance 82F/g, capacity retention 67.2%.Sample
Product WHBC-R and WHBC-S conservation rate in 10A/g capacitor has respectively reached 52.6% and 72.4%, though WHBC-S show it is good
Good capacity retention, but its specific capacitance value under 1A/g current density is only 98F/g.
In order to further inquire into the transmission dynamics of electrode interior to be measured, ac impedance measurement is carried out to three samples, is handed over
Flow impedance (EIS) can be reacted and the kinetic parameter in electric double layer capacitance, exchange with the faradaic electrochemical inside test material
Impedance test results are as shown in Figure 10；By 5.2 contents it is found that the chemical property of WHBC-L be it is best, it is similar by two
WHBC-L electrode assembling tests chemical property under double electric grade systems at the supercapacitor of symmetric double electricity grade；Symmetric double
GCD curve of the electric grade under different current densities is as shown in figure 11.
As seen from Figure 11, specific capacitance of the symmetric capacitor under 0.5A/g current density is 63F/g, with test electricity
The raising of current density, specific capacitance gradually decrease, and specific capacitance when 10A/g is 41F/g, capacity retention 65%.
The energy density and power density for having further calculated symmetric capacitor, the results are shown in Table 1, as can be seen from Table 1,
When power density is 0.035W/kg, energy density highest is 4.375Wh/kg.
1 the surveyed electrochemistry relevant parameter of WHBC-L symmetrical twin electrodes system of table
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the present invention, all in the spirit and principles in the present invention
Any modifications, equivalent replacements, and improvements done in range, should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of water hyacinth biomass carbon, it is characterised in that: the following steps are included:
S1, pretreatment: choosing mature living body water hyacinth, and removal jaundice, withered blade are repeatedly rushed with clean tap water
It washes, washes away the impurity and sludge on water hyacinth surface；
S2, drying: air-dried surface moisture after washed water hyacinth is cleaned 3-5 times with deionized water is put into baking oven, in 60-
4h is dried under the conditions of 100 DEG C, is then crushed with pulverizer, 60 mesh aperture sieves are crossed, and pack is stand-by；
S3, charing: smashed water hyacinth sample being put into crucible, and KCl and NaCl is completely covered on water hyacinth sample,
It covers crucible lid to be put into Muffle furnace, be warming up to 800 DEG C step by step and keep 3-4h；
S4, it is naturally cooling to room temperature to Muffle furnace, takes out crucible, the water hyacinth sample after charing is impregnated in 1MHCl solution
Then 2-3h with the multiple washed product of deionized water and filter until the aqueous solution pH filtered is 7, after suction filtration by filter membrane and
Sample is separated with filter membrane after dry in 120 DEG C of vacuum drying 6h, water hyacinth biomass carbon can be obtained, to water hyacinth by sample
Biomass carbon sample is weighed, and is saved backup.
2. a kind of preparation method of water hyacinth biomass carbon according to claim 1, it is characterised in that: the KCl and
NaCl ratio is 1:1.
3. a kind of preparation method of water hyacinth biomass carbon according to claim 1, it is characterised in that: the water hyacinth sample
The ratio of product and KCl and NaCl salt-mixture is 1:5.
4. a kind of preparation method of water hyacinth biomass carbon according to claim 1, it is characterised in that: the KCl and
The coverage mode of NaCl is first to be uniformly mixed the two, then be covered on water hyacinth sample.
5. a kind of preparation method of water hyacinth biomass carbon according to claim 1, it is characterised in that: in the step S2
Dry temperature is 80 DEG C.
6. a kind of preparation method of water hyacinth biomass carbon according to claim 1, it is characterised in that: in the step S1
Chosen material is the blade position of mature water hyacinth.
7. a kind of preparation method of water hyacinth biomass carbon according to claim 1, it is characterised in that: in the step S3
The rate of heating is 10 DEG C/min.
8. a kind of application of the water hyacinth biomass carbon of the method preparation as described in claim 1-7, which is characterized in that be applied to
Prepare electrode of super capacitor, comprising the following steps:
A, the steel wire of 500 mesh is cut into the strip of 12cm × 1.5cm, be cleaned by ultrasonic 3h with 6M NaOH and impregnates 12h, is used
30min is cleaned with EtOH Sonicate after ultrapure water, is placed in baking oven in 60 DEG C of drying 3h, flash is trimmed and remembers upper label, weighing
Record, sealing storage are stand-by；
B, the adhesive of the water hyacinth biomass samples of 80wt%, the conductive agent of 15wt% and 5wt% is taken to mix and grind in ethanol
Uniformly, ground sample is uniformly coated on to one end of ready steel wire, is obtained in 60 DEG C of vacuum drying 3h super
Capacitor working pole.
9. a kind of application of water hyacinth biomass carbon according to claim 8, it is characterised in that: described adhesive is poly- inclined
Vinyl fluoride.
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| CN110756167A (en) * | 2019-12-04 | 2020-02-07 | 河南师范大学 | Preparation method and application of modified biochar for adsorbing cadmium ions in wastewater |
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