CN107871869A - Adulterate the preparation method and applications of sisal fiber Quito pore carbon electrode material - Google Patents
Adulterate the preparation method and applications of sisal fiber Quito pore carbon electrode material Download PDFInfo
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- CN107871869A CN107871869A CN201710877324.7A CN201710877324A CN107871869A CN 107871869 A CN107871869 A CN 107871869A CN 201710877324 A CN201710877324 A CN 201710877324A CN 107871869 A CN107871869 A CN 107871869A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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
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Abstract
The invention discloses a kind of preparation method and applications for adulterating sisal fiber Quito pore carbon electrode material.Using sisal fiber as carbon source, by adding the form nitrogen doped of carbazole compound, doping sisal fiber base porous carbon material is prepared.Preparation method of the present invention is simple, mild condition；Prepared doping sisal fiber Quito pore carbon electrode material can replace the carbon material in the cathode lead plaster of part lead carbon battery, and the chemical property of lead carbon battery can be greatly improved.
Description
Technical field
The present invention relates to electrode material technical field, is related to a kind of preparation for adulterating sisal fiber Quito pore carbon electrode material
Method and its application, more particularly to a kind of preparation method and applications of carbazole doping sisal fiber Quito pore carbon electrode material.
Background technology
In recent years, the continuous development of China's automobile industry.Data are shown by the end of the year 2016, national vehicle guaranteeding organic quantity
Up to 2.9 hundred million, it is 5 times in 2007, is sure to occupy the second in the world.Due to largely using the non-renewable natural calculus-dissolving energy
As power source, caused vehicle exhaust is to cause one of city haze and the major reason of air pollution.In order to avoid not
The pollution that regenerative resource is brought to environment, therefore, greatly develop that new-energy automobile is imperative, such as the electronic vapour of energy-saving and emission-reduction
Car.And how electric vehicle industrialization key is caused to be whether the performance of battery has good effect.Lead carbon battery is lead
The product of both fusions of sour battery and ultracapacitor, has the high-energy-density of lead-acid battery and the Gao Gong of ultracapacitor concurrently
Two advantages of rate density.It can utilize in the field for needing the conventional batteries such as fast charging and discharging, long-term charge less electricity not use.Separately
Outside, the technique of lead carbon battery is similar to the production technology of existing lead-acid battery, and industrialization difficulty is not very big.With research
Further deeply, the first choice that following lead carbon battery turns into the electric powered motor energy because possessing the advantages such as high performance-price ratio.Just at present
For, still there are two hang-ups to hinder promoting the use of for lead carbon battery.It is battery first in partial state of charge high power charging-discharging
（HRPSoC）Worked under pattern, the irreversible sulfation phenomenon of lead carbon battery negative pole is extremely serious, next to that hydrogen evolution phenomenon is not easy
Solve, cause the cycle life of lead carbon battery to shorten.
Biological carbon material has the characteristics of cheap, abundance and reusable edible, is widely applied to energy and turns
Change and energy storage field.Sisal fiber is South China as a kind of natural tropical crops, the main place of production, have growth it is fast,
The features such as yield is high.Guangxi is one of main place of production for planting sisal fiber.According to incompletely statistics, the life of Guangxi District sisal fiber
Yield reaches the 80% of national total amount.Therefore, how to make good use of the attached value of sisal fiber and raising sisal fiber is to be worth pass
The problem of note.
Carbon material has good capacitive properties and higher conductance, with Pb/PbSO in lead carbon battery4Work
Potential matches, while also has good compatibility with lead active material, and carbon material is in PbSO caused by battery discharge procedure4
Conductive network is formd between crystal, promotes the reduction of lead, it is suppressed that PbSO4The reunion of crystal grain.Therefore, lead carbon battery with
Lead-acid accumulator compares, in high rate partial state of charge（HRPSoC）Lower circulation, the irreversible sulfation phenomenon of negative pole occurs
It is greatly improved, but still the problems such as a certain degree of sulfation, liberation of hydrogen is present, which prevent lead carbon battery industrialization
Process.Document shows that nitrogen-atoms adulterates in ultracapacitor can cause extra fake capacitance effect, and addition nitrogen-atoms is simultaneously
The wettability between electrode and electrolyte can be lifted, strengthens the transmittability of electrolyte ion and improves leading for carbon material
Electrically.Therefore doping heteroatom can strengthen the high rate performance of battery.Carbon is in adjacent position with nitrogen in periodic table
Put, and carbon atom is close with the electronegativity of nitrogen-atoms, two atomic radiuses are more or less the same, and material distortion is smaller after doping, so
Nitrogen-atoms is easier to be entrained in carbon material.It can suppress hydrogen evolution phenomenon to a certain extent using the carbon material of nitrogen atom doping
Occur, because the electronegativity of nitrogen-atoms is more bigger than carbon atom, cause carbon atom electron deficient, so as to weaken the generation of hydrogen.
The content of the invention
It is an object of the invention to provide a kind of preparation method and applications for adulterating sisal fiber Quito pore carbon electrode material.
Concretely comprise the following steps：
（1）Sisal fiber is cut into 1 cm with scissors, by the hydrogen-oxygen that the mass percent concentration prepared is 5 %
Change sodium solution, which is poured into sisal fiber, to be soaked 24 hours, then is soaked with the phosphoric acid solution that the mass percent concentration prepared is 5 %
Bubble 24 hours；After having soaked, sisal fiber therefrom being pulled out, being put into baking oven and dry 8 hours, temperature is 90 DEG C.
（2）Sisal fiber obtained by step (1) is put into sealed grinder and is ground, is ground into 300-400 mesh
Sisal fiber powder.
（3）Sisal fiber powder and 0.3 g carbazoles obtained by 8g steps (2) is weighed to be dissolved in 30 mL absolute ethyl alcohols,
Heated while stirring at 90 DEG C and obtain mixture completely to ethanol volatilization.
(4) mixture obtained by step (3) is placed in tube furnace and carbonized, 400 DEG C of heating 1 under the atmosphere of N 2
Hour, 1 hour is incubated, the wherein flow controls of N 2 are 100 mL/min, and programming rate is 10 DEG C/min.
（5）Step (4) gains are cooled to room temperature, are 1 according to step (4) gains and KOH mol ratios:3 ratio
Example weighs KOH, and step (4) gains are mixed with KOH, and adds 30mL deionized waters, is transferred in beaker, is put into baking oven,
Dried 24 hours at 110 DEG C；Transfer them in tube furnace, under 250-750 DEG C of activation temperature, in the atmosphere of N 2
Activate, then be incubated 1 hour within 1 hour.
（6）Step (5) the gains salt acid elution that 30 mL concentration are 0.1 mol/L, is transferred to vacuum drying chamber
In, 110 DEG C are heated 1 hour, are washed with deionized to cleaning solution pH=7, then are dried 8 hours at 105 DEG C, are mixed
Miscellaneous sisal fiber Quito pore carbon electrode material.
Adulterating sisal fiber Quito pore carbon electrode material can be instead of the carbon material in the cathode lead plaster of part lead carbon battery, energy
The chemical property of lead carbon battery is greatly improved.
Preparation method of the present invention is simple, mild condition；Using sisal fiber as carbon source, by the form for adding carbazole compound
Nitrogen doped, sisal fiber base porous carbon material is adulterated to prepare, doping sisal fiber base porous carbon material is placed in lead plaster
In, simulation lead carbon battery is assembled into, determines its first charge-discharge curve, cycle life, the results showed that, and undoped with sisal fiber
Base porous carbon material is compared, and the negative material containing doping sisal fiber base porous carbon material, has preferably charge-discharge performance,
Charging voltage is higher, and discharge platform is wider, and specific capacity is bigger, and this explanation adds doping sisal fiber base porous carbon in lead plaster
Material, has certain inhibitory action to the irreversible sulfation of lead carbon battery negative pole and hydrogen evolution phenomenon.
Brief description of the drawings
Fig. 1 is that the ESEM of doping sisal fiber Quito pore carbon electrode material prepared in the embodiment of the present invention shines
Piece.
Fig. 2 is the cyclic voltammogram of doping sisal fiber Quito pore carbon electrode material prepared in the embodiment of the present invention.
Fig. 3 is the electrochemical ac resistance of doping sisal fiber Quito pore carbon electrode material prepared in the embodiment of the present invention
Anti- spectrogram.
The grading curve of prepared doping sisal fiber Quito pore carbon electrode material in Fig. 4 embodiment of the present invention
Figure.
The BET adsorption/desorptions of prepared doping sisal fiber Quito pore carbon electrode material are bent in Fig. 5 embodiment of the present invention
Line chart.
Fig. 6 is that the lead plaster that doping sisal fiber Quito pore carbon electrode material prepared in the embodiment of the present invention makes is work
Make the first charge-discharge curve map of electrode.
Fig. 7 is that the lead plaster that doping sisal fiber Quito pore carbon electrode material prepared in the embodiment of the present invention makes is work
Make the cycle life curve map of electrode.
Embodiment
With reference to specific embodiment, the present invention is furture elucidated, but embodiment is not intended to limit protection scope of the present invention.
Embodiment:
（1）Sisal fiber is cut into 1 cm with scissors, by the hydroxide that the mass percent concentration prepared is 5 %
Sodium solution, which is poured into sisal fiber, to be soaked 24 hours, then is soaked with the phosphoric acid solution that the mass percent concentration prepared is 5 %
24 hours；After having soaked, sisal fiber therefrom being pulled out, being put into baking oven and dry 8 hours, temperature is 90 DEG C.
（2）Sisal fiber obtained by step (1) is put into sealed grinder and is ground, is ground into 300-400 mesh
Sisal fiber powder.
（3）Sisal fiber powder and 0.3 g carbazoles obtained by 8g steps (2) is weighed to be dissolved in 30 mL absolute ethyl alcohols,
Heated while stirring at 90 DEG C and obtain mixture completely to ethanol volatilization.
(4) mixture obtained by step (3) is placed in tube furnace and carbonized, 400 DEG C of heating 1 under the atmosphere of N 2
Hour, 1 hour is incubated, the wherein flow controls of N 2 are 100 mL/min, and programming rate is 10 DEG C/min.
（5）Step (4) gains are cooled to room temperature, are 1 according to step (4) gains and KOH mol ratios:3 ratio
Example weighs KOH, and step (4) gains are mixed with KOH, and adds 30mL deionized waters, is transferred in beaker, is put into baking oven,
Dried 24 hours at 110 DEG C；Transfer them in tube furnace, under 550 DEG C of activation temperatures, 1 is small in the atmosphere of N 2
When activate, then be incubated 1 hour.
（6）Step (5) the gains salt acid elution that 30 mL concentration are 0.1 mol/L, is transferred to vacuum drying chamber
In, 110 DEG C are heated 1 hour, are washed with deionized to cleaning solution pH=7, then are dried 8 hours at 105 DEG C, are mixed
Miscellaneous sisal fiber Quito pore carbon electrode material.
Adulterate ESEM, cyclic voltammetry curve figure, the electrochemical AC impedance of sisal fiber Quito pore carbon electrode material
Spectrogram, grading curve figure are shown in Fig. 1, Fig. 2, Fig. 3 and Fig. 4 respectively.
（7）The preparation of lead plaster：By step（6）Gained adulterates sisal fiber Quito pore carbon electrode material and negative electrode active material
（Lead powder 15, the g of lead oxide 3）, conductive agent（The g of acetylene black 0.15）, swelling agent（BaSO41.8 g）With liberation of hydrogen inhibitor
（Indium oxide, gallium oxide and each 0.09 g of zinc oxide）Mixing, add 6 mL polytetrafluoroethylene (PTFE)（PTFE）Emulsion and 6 mL
Secondary water, mechanical agitation 24 hours obtains lead plaster to generation pasty masses.
（8）Simulate the making of lead carbon battery：Will（7）In lead plaster be coated onto on plate railings of anode and cathode, smear uniform.Then will
Battery lead plate, which is placed in vacuum drying chamber, to be dried 12 hours, and temperature is 60 DEG C, obtains lead carbon battery positive-negative electrode plate.
76 mL distilled water and 1.28 g/cm is added in 100 mL beaker3Sulfuric acid, be made needed for electrolyte, will be positive and negative
Pole plate insertion beaker both sides, centre are separated with the AGM dividing plates of industrial used in battery, produce simulation lead carbon battery, by its with
LAND5.8 battery test systems are connected, and switch on power, and are melted into.The effect of chemical conversion is by the active material PbO of positive pole
It is converted into PbO2, secondly, the lead of negative electrode active material is converted into spongy lead, this be due to spongy lead activity very
Height, possesses loose structure.The final purpose of chemical conversion is to allow material and electrolyte fully to merge, and positive reaction and back reaction reach
To an equalization point, discharge and recharge is a stable cyclic process when battery is subsequently used, you can obtains qualified both positive and negative polarity
Plate.
Fig. 6 is that the lead plaster that doping sisal fiber Quito pore carbon electrode material prepared in the embodiment of the present invention makes is work
Make the first charge-discharge curve map of electrode, Fig. 7 is doping sisal fiber Quito pore carbon electrode prepared in the embodiment of the present invention
The lead plaster that material makes is the cycle life curve map of working electrode.Analysis chart 6 is understood, containing undoped with sisal fiber Quito hole
For the negative material of Carbon Materials compared with the negative material containing doping sisal fiber base porous carbon material, the latter has higher fill
Piezoelectric voltage, possess longer discharge platform, and discharge platform voltage is higher, termination capacity reaches 84.0 mAh/g, and containing not
The negative material termination capacity for adulterating sisal fiber base porous carbon material is 73.6 mAh/g, contains doping sisal fiber Quito
The battery performance of the negative material assembling of hole Carbon Materials improves 14.13 %.Because due to the doping of nitrogen-atoms, carbon materials
The surface of material and bigger conductive network system is internally formed, has been advantageous to the infiltration of electrolyte and electronics in charge and discharge process
Transmission.In addition, the addition of nitrogen-atoms can make the utilization rate of negative electrode active material be improved to some extent, there is provided bigger counterfeit electricity
Hold effect, while improve the stability and discharge performance of electrochemical reaction process.Analysis chart 7 understands that different negative materials exist
After circulation 160 times, the percentage of theoretical capacity shared by capacity is different, contains doping sisal fiber porous carbon materials
Negative material specific capacity accounts for the 70.5% of initial specific capacity, and contains the negative material undoped with sisal fiber base porous carbon material
Account for 49.8%.So containing doping sisal fiber base porous carbon material negative material assembling battery have good efficiency with
And cycle performance.This has good boundary mainly due between doping carbazole sisal fiber base porous carbon material and active material
Face compatibility, greatly improve the utilization rate of active material, therefore specific capacity is higher, possesses good cycle performance.
Claims (2)
1. a kind of preparation method for adulterating sisal fiber Quito pore carbon electrode material, it is characterised in that concretely comprise the following steps：
（1）Sisal fiber is cut into 1 cm with scissors, by the hydrogen-oxygen that the mass percent concentration prepared is 5 %
Change sodium solution, which is poured into sisal fiber, to be soaked 24 hours, then is soaked with the phosphoric acid solution that the mass percent concentration prepared is 5 %
Bubble 24 hours；After having soaked, sisal fiber therefrom being pulled out, being put into baking oven and dry 8 hours, temperature is 90 DEG C；
（2）Sisal fiber obtained by step (1) is put into sealed grinder and is ground, is ground into the sword of 300-400 mesh
Flaxen fiber powder；
（3）Sisal fiber powder and 0.3 g carbazoles obtained by 8g steps (2) is weighed to be dissolved in 30 mL absolute ethyl alcohols,
Heated while stirring at 90 DEG C and obtain mixture completely to ethanol volatilization；
(4) mixture obtained by step (3) is placed in tube furnace and carbonized, 400 DEG C of heating 1 are small under the atmosphere of N 2
When, 1 hour is incubated, the wherein flow controls of N 2 are 100 mL/min, and programming rate is 10 DEG C/min；
（5）Step (4) gains are cooled to room temperature, are 1 according to step (4) gains and KOH mol ratios:3 ratio claims
KOH is taken, step (4) gains are mixed with KOH, and adds 30mL deionized waters, is transferred in beaker, is put into baking oven,
Dried 24 hours at 110 DEG C；Transfer them in tube furnace, under 250-750 DEG C of activation temperature, 1 is small in the atmosphere of N 2
When activate, then be incubated 1 hour；
（6）Step (5) the gains salt acid elution that 30 mL concentration are 0.1 mol/L, is transferred in vacuum drying chamber, 110
DEG C heating 1 hour, be washed with deionized to cleaning solution pH=7, then at 105 DEG C dry 8 hours, obtain adulterate sisal hemp
Fiber-based porous carbon electrode material.
2. the application of doping sisal fiber base porous charcoal according to claim 1, it is characterised in that described doping sisal hemp
Fiber-based porous charcoal can be used as and prepare electrode material application.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110707302A (en) * | 2019-10-14 | 2020-01-17 | 桂林理工大学 | Preparation method and application of sisal fiber carbon/lead composite material |
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Application publication date: 20180403 Assignee: GUANGXI CHAOXING SOLAR ENERGY TECHNOLOGY Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000497 Denomination of invention: Preparation and Application of Doped Sisal Fiber Based Porous Carbon Electrode Materials Granted publication date: 20191011 License type: Common License Record date: 20221229 |
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