CN110589823A - Shaddock peel porous carbon material and preparation method and application thereof - Google Patents
Shaddock peel porous carbon material and preparation method and application thereof Download PDFInfo
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- CN110589823A CN110589823A CN201910615650.XA CN201910615650A CN110589823A CN 110589823 A CN110589823 A CN 110589823A CN 201910615650 A CN201910615650 A CN 201910615650A CN 110589823 A CN110589823 A CN 110589823A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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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- 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 invention discloses a shaddock peel porous carbon material and a preparation method and application thereof, and relates to an electrode material. The preparation method of the carbon material comprises the following steps: 1) placing the shaddock peel in a tubular furnace, introducing nitrogen for 20-40 min, heating to 440-460 ℃ at the speed of 1-3 ℃/min, carbonizing for 1-3 h, and naturally cooling to obtain carbonized shaddock peel; 2) mixing carbonized shaddock peel and KOH according to the mass ratio of 1: 1-4, grinding, putting into a tubular furnace, introducing nitrogen for 20-40 min, heating to 790-810 ℃ at the speed of 1-3 ℃/min, activating for 1-3 h, and naturally cooling to obtain activated shaddock peel; 3) and (3) adjusting the pH value of the activated shaddock peel to 10, centrifuging, performing vacuum filtration, washing, and drying in a forced air drying oven to obtain the shaddock peel porous carbon material.
Description
Technical Field
The invention relates to an electrode material, in particular to a shaddock peel porous carbon material and a preparation method and application thereof.
Background
With the progress of scientific technology, the development of social economy and the rapid increase of population, the consumption of energy is more and more, the exhaustion of non-renewable resources urgently requires renewable resources to play a role in substitution, and simultaneously requires sustainable and effective utilization of the non-renewable resources to fully play the potential of the non-renewable resources. The existing traditional energy system can not meet the development requirements of modern industry, agriculture, forestry and the like, and fuel oil and coal carbon resources are not only non-renewable, but also can generate a large amount of CO in the use and consumption process2、SO2And the like, which brings about serious environmental pollution. This has led to a greater emphasis on the establishment of new and effective energy supply systems to ensure a sustainable economic growth, while also providing environmental benefits.
Among them, the development of new energy and renewable clean energy is the most effective method for solving the problem at present, and is one of the key technologies that must be solved in the 21 st century, and the new energy material is the foundation and core for realizing the development and utilization of new energy and supporting the development thereof.
The battery industry is an important component of the new energy application field, since electrical energy has become an indispensable source for human production and social development as the ultimate form of energy utilization. The development of power supply has been thought of as lithium ion battery with high energy density, but when lithium battery is used as power supply, it has a obvious disadvantage that the power density is small, so that the requirement of high power discharge cannot be met, and this defect has become a main obstacle for limiting the development. Therefore, a super capacitor capable of being charged and discharged quickly becomes a new research hotspot, but the charge storage density of the super capacitor is too low to supply power for a long time, so that the application prospect of the super capacitor as a power supply is limited.
The super capacitor is a device between a traditional capacitor and a rechargeable battery, and has the characteristics of quick charge and discharge, environmental friendliness, high power density, ultra-long cycle life, no pollution, wide working temperature range and the like. At present, mainly metal oxides, conductive polymers, activated carbon materials, and many doped composite materials are used as electrode materials thereof. The capacitor using the activated carbon as the electrode material has a long research history and the technology is the most mature, but the production process is complex, the production period is long, the capacity is generally low, and the application of the super capacitor is limited.
Disclosure of Invention
The invention aims to provide a shaddock peel porous carbon material, a preparation method and application thereof.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a preparation method of a shaddock peel porous carbon material comprises the following steps:
1) placing the shaddock peel in a tubular furnace, introducing nitrogen for 20-40 min, heating to 440-460 ℃ at the speed of 1-3 ℃/min, carbonizing for 1-3 h, and naturally cooling to obtain carbonized shaddock peel;
2) mixing carbonized shaddock peel and KOH according to the mass ratio of 1: 1-4, grinding, putting into a tubular furnace, introducing nitrogen for 20-40 min, heating to 790-810 ℃ at the speed of 1-3 ℃/min, activating for 1-3 h, and naturally cooling to obtain activated shaddock peel;
3) and (3) adjusting the pH value of the activated shaddock peel to 10, centrifuging, performing vacuum filtration, washing, and drying in a forced air drying oven to obtain the shaddock peel porous carbon material.
The introduction time of nitrogen in the step 1) is 30min, and the carbonization time is 2 h.
In the step 1), the heating rate is 2 ℃/min, and the target temperature is 450 ℃.
And 2) grinding by using an agate mortar.
The introduction time of nitrogen in the step 2) is 30min, and the activation time is 2 h.
The reagent used for adjusting the pH value in the step 3) is KOH.
The centrifugation speed in the step 3) is 7000r/min, and the centrifugation time is 5 min.
The washing solvent in the step 3) is HCl and deionized water.
The drying temperature in the step 3) is 80 ℃.
A porous carbon material of shaddock peel, which is prepared by the method of any one of claims 1 to 9.
The shaddock peel porous carbon material as claimed in claim 9, applied to electrode fabrication and assembly, namely:
firstly, ultrasonically washing foamed nickel with deionized water and ethanol in sequence, drying, weighing, then mixing the prepared sample with polyvinylidene fluoride and acetylene black according to the mass ratio of 0.85:0.05:0.15, adding N-methyl pyrrolidone for size mixing, coating the mixture on foamed nickel with the thickness of 2 x 1cm, then placing the foamed nickel in a vacuum drying oven for drying at the temperature of 80 ℃ for about 6 hours, tabletting on a table type electric tablet press under the pressure of 10MPa, weighing the mass of the foamed nickel again, and obtaining the mass of an active substance by 85% of the mass difference of two times. Taking foamed nickel coated with active substances as a working electrode, foamed nickel as a counter electrode and an HgO/Hg electrode as a reference electrode to form a three-electrode system, soaking in 6MKOH for 3 hours, and introducing 10min N into an electrolytic cell before testing2Exhaust O2。
Compared with the prior art, the invention has the following beneficial effects:
the preparation processes of graphene and carbon nanotubes are both relatively complex. Currently, as for the production of graphene, there are mainly physical production methods (mechanical exfoliation method, explosion method, orientation and adhesion method, etc.) and chemical production methods (electrochemical method, chemical vapor deposition method, graphite intercalation method, graphite oxide reduction method, etc.) in the literature. As for the production of carbon nanotubes, catalytic pyrolysis, flame method, template method, arc discharge method, condensed phase electrolysis method, laser evaporation method, and the like are mainly cited in the literature. No matter which method is adopted, the preparation process is relatively complex, and the repeatability of the physicochemical characteristics of part of the product is poor due to the fact that part of conditions are difficult to accurately control.
Most of carbonaceous materials have poor hydrophilicity, and the electric double layer capacitance formed by the carbonaceous materials in the electrode materials is reduced to a certain extent. Carbon materials containing heteroatoms (e.g., N, S, B, etc.), especially N-containing carbon materials, have attracted many researchers' interest because they enhance charge asymmetry and induce structural deformation, which increases the electron transport ability of the material itself.
The invention provides a method which is simple to operate and easy to control. The pomelo is a common fruit in China, the pomelo peel accounts for 44-55% of the total mass of the pomelo, but the peel of the pomelo is not well utilized after the pomelo is eaten. Because of its large amount of fluffy fibrous structure and pectin, if activated to prepare a porous carbon material, it will provide many hydrophilic groups to the material. Therefore, the research uses the shaddock peel as a raw material to prepare the cathode material of the super capacitor, and is expected to be applied in a large scale.
According to the invention, shaddock peel is taken as a raw material, carbonized at 450 ℃ for 2 hours, and then calcined at 800 ℃ for 2 hours by using KOH as an activating agent according to the carbon-alkali ratio of 1:1 to prepare the high specific capacitance super capacitor cathode material, the specific capacitance of the high specific capacitance super capacitor cathode material reaches 357.6F/g, and the specific capacitance retention rate reaches more than 90% after 3000 cycles. The preparation method is simple and convenient, the raw materials are easy to obtain and cheap, and the prepared material has excellent performance, not only can solve the problem of low recycling rate of the shaddock peel, but also can be used for preparing the material with high electrochemical performance.
Drawings
FIG. 1 is a flow chart for manufacturing porous carbon material of shaddock peel;
FIG. 2 is a plot of cyclic voltammograms at 5mV/s scan rate for activated samples of different ratios;
FIG. 3 is a constant current charge and discharge curve at 0.5A/g current density for different samples;
FIG. 4 is a graph of a representative cyclic voltammogram of a pH1 sample at a scan rate of 5-100 mV/s;
FIG. 5 is a constant current charge and discharge curve diagram of a PH1 sample at a current density of 0.5-5A/g;
FIG. 6 is a graph of cycle life at 1A/g current density for a PH1 sample;
FIG. 7 is a scanning electron micrograph of pericarpium Citri Grandis; wherein, (a) scanning electron microscope images of unactivated shaddock peel and (b) scanning electron microscope images of PH1 sample.
Detailed Description
The invention is further defined in the following detailed description of the claims, which are to be read in connection with the following examples, which are not to be construed as limiting the invention in any way.
Example 1
Preparing shaddock peel charcoal:
placing 5g of shaddock peel in a porcelain boat, placing in a tube furnace, introducing nitrogen for 30min, heating to 450 ℃ at the speed of 2 ℃/min under the protection of nitrogen, carbonizing for 2 hours, and naturally cooling to obtain carbonized shaddock peel. The carbonized pomelo peel is mixed with KOH according to a certain mass ratio (m (carbonized pomelo peel): m (KOH): 1, 1:2, 1:3, 1:4) and is named as PH1, PH2, PH3, PH4 in sequence. And then, respectively putting each sample into an agate mortar for grinding, then putting the sample into a tube furnace, introducing 30min of nitrogen, heating to 800 ℃ at the speed of 2 ℃/min under the protection of the nitrogen, activating for 2 hours, and then naturally cooling. Adding 6M KOH into the activated material, adjusting pH to about 10 (since alkali can corrode the porcelain boat, adding alkali liquor to dissolve corroded substances on the inner wall of the porcelain boat mixed in the material), centrifuging in a centrifuge at the rotating speed of 7000r/min for 5min, performing vacuum filtration, washing with deionized water, washing with 1M HCl to pH of about 7, and washing with deionized water to remove Cl-And K+. Finally, the activated material is put into a blast drying oven to be dried at 80 ℃.
The above samples were tested for performance, as detailed in FIGS. 2-7, wherein:
FIG. 2 is a plot of cyclic voltammetry at 5mV/s for different mass ratios of KOH-activated porous carbon material, from which it can be seen that the curves for all four samples resemble rectangles, while exhibiting excellent electrochemical performance. In addition, the rectangular area of the PH1(m (carbonized pomelo peel): m (koh): 1) material is the largest, indicating that the larger the mass specific capacitance of the material is
As shown in FIG. 3, the constant current charging and discharging curve of different samples at 0.5A/g is shown, at this time, the PH1 sample still has longer charging and discharging time than the other three samples, the curve of each sample presents a linear relationship better, the charging and discharging curves and the time axis enclose an approximate isosceles triangle, and the excellent symmetry of the material during charging and discharging is reflected. From the data in the third figure, the mass specific capacitance of the four materials was calculated by using equation (1), and the calculation results are shown in Table 1, where the mass specific capacitance of the PH1 sample reached 357.6F/g. The mass specific capacitance is continuously reduced with the increase of the alkali dosage.
Further cyclic voltammetry measurements on the PH1 sample are shown in FIG. 4, which is a cyclic voltammetry graph of the PH1 sample at a scan rate of 5-100 mV/s, and shows that the curves of the PH1 sample all present a regular rectangular-like shape before a scan rate of 80mV/s, while at scan rates greater than 80mV/s, the material is slightly polarized.
Fig. 5 is a graph showing the charge and discharge curves of the PH1 sample at different current densities, in which the curves still have good linear relationship and symmetrical triangular shapes at different current densities, and the sudden change of the curves is small near the inflection point of charge and discharge at high current, which indicates that the polarization phenomenon is small even in large current charge and discharge.
FIG. 6 is a graph of the cycle life of a PH1 sample at a current density of 1A/g. After 3000 times of circulation, the material can still maintain the specific capacitance of more than 90%, and in addition, when the material is charged and discharged for less than 500 times, the specific capacitance slightly decreases, then increases, and even exceeds the initial specific capacitance.
Fig. 7(a) is a Scanning Electron Microscope (SEM) image of shaddock peel without alkali activation, and fig. 7(b) is an SEM image of a PH1 sample. By contrast, the surface of the shaddock peel has a layered structure when the shaddock peel is not activated, and the layered structure of the shaddock peel after activation is still maintained, as shown by the red circles in fig. 7. In addition, the activated material has a plurality of nano-spheres with the diameter of about 30nm, as shown by the circles of yellow dotted lines in FIG. 7(b), and a plurality of holes are formed among the spheres, so that the intercalation and deintercalation of electrolyte ions are greatly facilitated.
The results of the bench electron microscope spectroscopy integrated machine on the content of C, O, N element in the material are shown in table 2. Comparing the O content/C content of the two materials, the O content of the PH1 sample is obviously increased, which means that more oxygen-containing functional groups such as carboxyl, hydroxyl, carbonyl and the like are possibly introduced into the surface of the material, so that the hydrophilicity of the material can be improved, the adsorbability and wettability of the electrode material and an electrolyte are improved, and the specific capacitance of the material is finally improved.
Example 2
Electrode manufacturing and assembling:
firstly, ultrasonically washing foamed nickel with deionized water and ethanol in sequence, drying, weighing the foamed nickel, and then mixing the prepared sample with polyvinylidene fluoride and acetylene black according to a mass ratio of 0.85:0.05:0.15, adding N-methyl pyrrolidone, mixing, coating on 2 multiplied by 1cm of foamed nickel, drying in a vacuum drying oven at 80 ℃ for about 6 hours, tabletting on a table type electric tablet press under the pressure of 10MPa, weighing the mass of the foamed nickel again, wherein 85% of the mass difference of the two times is the mass of the active substance. Taking foamed nickel coated with active substances as a working electrode, foamed nickel as a counter electrode and an HgO/Hg electrode as a reference electrode to form a three-electrode system, soaking in 6MKOH for 3 hours, and introducing 10min N into an electrolytic cell before testing2Exhaust O2。
Claims (10)
1. A preparation method of a shaddock peel porous carbon material is characterized by comprising the following steps:
1) placing the shaddock peel in a tubular furnace, introducing nitrogen for 20-40 min, heating to 440-460 ℃ at the speed of 1-3 ℃/min, carbonizing for 1-3 h, and naturally cooling to obtain carbonized shaddock peel;
2) mixing carbonized shaddock peel and KOH according to the mass ratio of 1: 1-4, grinding, putting into a tubular furnace, introducing nitrogen for 20-40 min, heating to 790-810 ℃ at the speed of 1-3 ℃/min, activating for 1-3 h, and naturally cooling to obtain activated shaddock peel;
3) and (3) adjusting the pH value of the activated shaddock peel to 10, centrifuging, performing vacuum filtration, washing, and drying in a forced air drying oven to obtain the shaddock peel porous carbon material.
2. The preparation method of the shaddock peel porous carbon material as claimed in claim 1, wherein the nitrogen gas is introduced for 30min and the carbonization time is 2h in the step 1).
3. The method for preparing the shaddock peel porous carbon material as recited in claim 1, wherein the temperature increase rate in the step 1) is 2 ℃/min, and the target temperature is 450 ℃.
4. The method for preparing the shaddock peel porous carbon material as claimed in claim 1, wherein the grinding in step 2) is performed using an agate mortar.
5. The preparation method of the shaddock peel porous carbon material as claimed in claim 1, wherein the nitrogen gas is introduced for 30min and the activation time is 2h in the step 2).
6. The method for preparing the shaddock peel porous carbon material as recited in claim 1, wherein the agent for adjusting the pH in the step 3) is KOH, and the washing solvent is HCl and deionized water.
7. The method for preparing the shaddock peel porous carbon material as recited in claim 6, wherein the centrifugation speed in the step 3) is 7000r/min and the centrifugation time is 5 min.
8. The method for preparing the shaddock peel porous carbon material as recited in claim 7, wherein the drying temperature in the step 3) is 80 ℃.
9. A porous carbon material of shaddock peel, characterized by being produced by the method of any one of claims 1 to 9.
10. The shaddock peel porous carbon material as claimed in claim 9, applied to electrode fabrication and assembly.
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Cited By (3)
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| CN111204734A (en) * | 2020-01-20 | 2020-05-29 | 上海应用技术大学 | Flaky biomass carbon material and preparation method thereof |
| CN112875701A (en) * | 2020-07-04 | 2021-06-01 | 山东八三石墨新材料厂 | Preparation method and application technology of biomass carbon supercapacitor electrode material |
| CN113184848A (en) * | 2021-04-22 | 2021-07-30 | 合肥工业大学 | Method for preparing biomass porous carbon for supercapacitor based on shaddock peel |
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