CN107311172A - A kind of passion fruit shell base porous carbon materials and its preparation method and application - Google Patents
A kind of passion fruit shell base porous carbon materials and its preparation method and application Download PDFInfo
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2006/17—Pore diameter distribution
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Abstract
The invention discloses a kind of passion fruit shell base porous carbon materials, by passion fruit shell handled through low-temperature carbonization after mixed with nitrogen-containing compound, be prepared from using alkali inorganic substance calcining and activating, specific surface area scope is 1500 ~ 2603 m2 g‑1, pore-size distribution is homogeneous, is distributed in the range of 1.80 ~ 2.40 nm.Its preparation method includes：Step 1）The low-temperature carbonization of passion fruit shell；Step 2）The activation of passion fruit shell base carbon material；Step 3）The post processing of passion fruit shell base carbon material.Used as electrode material for super capacitor, when current density is 0.5 A g‑1When, specific capacitance value scope is 261 ~ 347 F g‑1.The present invention is carbon source from passion fruit shell, improves passion fruit shell resource comprehensive utilization ratio, obtains the product of high additive value.The material has good performance of the supercapacitor, such as good cyclical stability and high rate performance, is had broad application prospects in energy storage with conversion field.
Description
Technical field
The present invention relates to porous material technical field, and in particular to a kind of passion fruit shell Quito structure carbon material and its preparation side
Method and application.
Background technology
Ultracapacitor as a kind of new and effective energy storage device, with power density it is high, have extended cycle life, discharge and recharge effect
Rate is high, non-maintaining, energy-conserving and environment-protective etc. series of advantages, rapidly in electric automobile, electric power, railway, consumption electronic products etc.
Various fields are applied.At present, the electrode material that ultracapacitor is used mainly has three major types：Carbon-based material, metal oxidation
Thing and conducting polymer.Porous carbon materials in carbon-based material are the widest class electrode materials of current application, due to
Good physical and chemical performance, such as specific surface area are big, pore structure is controllable, chemical property is stable, high heat conduction, high conductivity and original
Expect abundant etc..Pursuit with people to environmental protection cleaning technology, biomass material is with its natural green, wide material sources and tool
The research object that having the features such as the pattern and carbonaceous structure of uniqueness turns into preparation porous carbon sill of sheet has obtained extensive concern.
Abandoned biomass is to prepare one of desirable feedstock of porous carbon, and porous carbon is prepared by raw material of abandoned biomass, can
Effectively reduce the directly burning of house refuse and discarded object and handle discharged carbon dioxide, while obtaining the porous carbon of high added value
Product, be it is a kind of turn waste into wealth, the method for carbon fixation and emission reduction and biomass as resources.Guangxi is the main production base of national passion fruit
Ground, the annual production of the whole city of Beiliu City passion fruit is up to more than 120,000 tons.Passion fruit shell has loose structure and substantial amounts of as accessory substance
Cellulose, lignin, these structures will not be destroyed during charing, therefore, be prepared by raw material of agricultural wastes
Porous carbon materials are by one of effective ways of recycling waste.Moreover, its bigger serface of biomass carbon material use
Physical characteristic, preferable electric double layer capacitance performance can be obtained.
Pure carbon material is directed to, the introducing hetero-atoms such as nitrogen-atoms in porous carbon materials, it is possible to increase the profit of material surface
Moist and stability, meanwhile, can occur reversible redox reaction to provide fake capacitance with electrolyte.Therefore, nitrogen is mixed
Miscellaneous porous carbon has high specific surface area, abundant pore structure and substantial amounts of surface nitrogen-containing functional group, so as to assign the material
The properties, the electrode material for making it be widely used in ultracapacitor such as unique machinery, electronics, energy storage.
The especially high specific surface area porous carbon micropore of porous carbon enriches, but specific surface area utilization rate is low, possible
Reason is the infiltration that too small micropore is unfavorable for electrolyte, causes electric charge not to be adsorbed, and is unfavorable for the formation of electric double layer, micropore
Also it is unfavorable for the diffusion and transmission of electric charge, influences the energy density and power density of capacitor.Li et al. using Chinese ash fallen leaves as
Raw material, with reference to KOH and K2CO3The porous carbon materials of aperture structure expansion are prepared, in 0.5 A g during as three electrode tests−1
Specific capacitance is up to 310 F g under current density−1[Journal of Power Sources 2015, 299, 519-528].Should
The cheap biomass of method selection is as carbon source, and synthetic method is simple.But the specific surface area of prepared porous carbon materials
Relatively low, specific capacity declines comparatively fast, in 5 A g at higher current densities−1Specific capacity under current density is only 240 F g−1.Cause
This, it is to improve super to carry out rationally control while exploitation high-specific surface area nitrogen-doped porous carbon material to the distribution of its aperture structure
One of the energy density of capacitor and the key technology of power density.
Based on above-mentioned consideration, expected from the shell of passion fruit as source, prepare biomass-based porous carbon materials, utilize its carbon
Its loose porous structure is remained after change, with larger specific surface area, and pore-size distribution and pore volume are within the specific limits
It is adjustable, it is a kind of preferable electrode material for super capacitor.
The content of the invention
It is an object of the invention to provide a kind of passion fruit shell base porous carbon materials and its preparation method and application, aperture is realized
While adjustable, high-specific surface area, lifting performance of the supercapacitor, waste's reclamation rate is improved, increase passion fruit shell
Economic value added, reduces electrode material production cost.
In order to realize foregoing invention purpose, the technical solution adopted by the present invention：Using passion fruit shell be carbon source, semicarbazides,
Urea or guanidine carbonate are nitrogen source, use alkali inorganic substance KOH etc. for activator, utilize stable three-dimensional many of chemical activation method synthesis
Hole carbon material.Nitrogen not only can be successfully entrained in carbon by semicarbazides, urea or guanidine carbonate as the nitrogen source of high nitrogen content
In material, pore creating material is also used as, with reference to KOH activators, the pore-size distribution of carbon material is adjusted, improves the nitrogen content of carbon material
And electric conductivity, so as to increase the specific surface area of material as far as possible, the electric double layer of large area is formed, the property of ultracapacitor is improved
Energy.
Realizing the concrete technical scheme of the object of the invention is：
Passion fruit shell base porous carbon materials, by passion fruit shell handled through low-temperature carbonization after mixed with nitrogen-containing compound, using alkalescence
Inorganic matter calcining and activating is prepared from, and its specific surface area scope is 1500 ~ 2603 m2 g-1, pore-size distribution is homogeneous, is distributed in
In the range of 1.80 ~ 2.40 nm.
The preparation method of passion fruit shell base porous carbon materials comprises the following steps：
Step 1）The low-temperature carbonization of passion fruit shell, passion fruit shell is cleaned, block, drying is cut into, be placed in Muffle furnace 300 ~
At a temperature of 450 DEG C, carbonized product is filtered, washed, dried, ground by the h of low-temperature carbonization 1 ~ 3, obtains passion fruit shell base carbon materials
Material；
Step 2）The activation of passion fruit shell base carbon material, by step 1）Gained passion fruit shell base carbon material and nitrogen-containing compound and alkali
Property inorganic matter in mass ratio be 1.0：（0.5~4.0）：（1.5~6.0）Mixing, after soaking in deionized water, puts pipe into after drying
In formula stove under nitrogen atmosphere protection, using activation temperature as 600 ~ 900 DEG C, soak time is that 1 ~ 6 h is condition, and calcining and activating is obtained
To nitrogen-doped modified passion fruit shell base carbon material, described nitrogen-containing compound is semicarbazides, urea or guanidine carbonate, described alkali
Property inorganic matter be potassium hydroxide, sodium hydroxide, potassium carbonate or zinc chloride；
Step 3）The post processing of passion fruit shell base carbon material, above-mentioned product is soaked with hydrochloric acid solution, by washing, filtering, is dried
Dry, grinding obtains passion fruit shell base porous carbon materials.
Passion fruit shell base porous carbon materials as electrode material for super capacitor application, when current density be 0.5 A g-1
When, specific capacitance value scope is 261 ~ 347 F g-1。
The scanned testing electronic microscope of passion fruit shell base porous carbon materials shows that the carbon material shows cellular many
Pore structure.
Passion fruit shell base porous carbon materials show that it has higher ratio table through adsorption isothermal curve and pore-size distribution test
Area, up to 2603 m2 g-1, substantial amounts of micropore and appropriate mesoporous, average pore size is 1.92 nm, and pore volume is 1.25cm3g-1。
Passion fruit shell base porous carbon materials show through constant current charge-discharge test, when current density is 0.5 A g-1When, than
Capacitance is up to 261 ~ 347 F g-1。
Passion fruit shell base porous carbon materials show through cyclic voltammetry, under different sweep speeds, and cyclic voltammetric is bent
Line keeps good and is similar to rectangular shape, shows there is the performance of good electric double layer capacitance.
Passion fruit shell base porous carbon materials show through constant current charge-discharge test result, in 20 A g-1Under high current density,
Specific capacitance value is up to 252 F g-1, specific capacitance conservation rate still has 88 % after being circulated at 10000 times.
In order to contrast the influence for whether adding nitrogen source to carbon material structure and performance, further synthesis is without the doping of additional nitrogen source
Passion fruit shell base porous carbon materials.Tested through adsorption isothermal curve and pore-size distribution test and constant current charge-discharge, as a result table
It is bright, without additional nitrogen source adulterate passion fruit shell based cellular structures carbon material have wider pore-size distribution, low specific surface area compared with
It is small（1505 m2 g-1）With less pore volume（0.73cm3g-1）, when current density is 0.5 A g-1When, specific capacitance value is 261 F
g-1。
Contrast test result shows that the passion fruit shell base porous carbon materials specific surface area and pore volume obtained after addition nitrogen source is equal
Increase, pore-size distribution are homogeneous, further enhancing its performance of the supercapacitor, and its specific capacity increases, followed under high current density
Ring performance is stable.
The passion fruit shell based cellular structures carbon material of the present invention is for prior art, with advantages below：
First, the present invention is carbon source from discarded passion fruit shell, improves passion fruit shell resource comprehensive utilization ratio, obtains high extra price
The product of value；
2nd, it is nitrogen source using semicarbazides in the present invention, it is decomposed in the condition of high temperature and advantageously forms more micropores, and can
Different types of nitrogen-atoms is mixed on carbon wall, more electric double layer capacitances and fake capacitance are provided for ultracapacitor；
3rd, biomass-based loose structure carbon material prepared by this method has high specific surface area, and scope is 1500 ~ 2603 m2
g-1, with abundant micropore and in right amount mesoporous, average pore size distribution is homogeneous, is distributed in the range of 1.80 ~ 2.40 nm, favorably
In increase specific surface area, so as to improve the performance of the double layer capacitor of ultracapacitor；
4th, as the application of electrode material for super capacitor, when current density is 0.5A g-1When, specific capacitance value scope 261 ~
347 F g-1, and with good cyclical stability and high rate performance.
The present invention prepares the limitation of nitrogen-doped carbon material technology for prior art, by new nitrogen source of semicarbazides,
Passion fruit shell be carbon source, at high temperature, alkali inorganic substance is performed etching to carbon material, formed micropore, etch produce gas with
And the decomposition of nitrogen source advantageously forms abundant pore structure and increase specific surface area, ultimately forms nitrogen-doped modified
Passion fruit shell base porous carbon materials.When it is used as electrode material for super capacitor, the micropore in porous carbon materials is mainly provided
Larger ratio surface, mesopore is the transmission channel of electrolyte ion, and macroporous structure can play a part of electrolyte buffer pool, real
The good high rate performance of electrode of super capacitor is showed, in 20 A g-1Current density under specific capacity remain at 252 F g-1。
Therefore, the present invention has broad application prospects in fields such as ultracapacitor, lithium ion batteries.
Brief description of the drawings：
Fig. 1 is the scanning electron microscopy picture figure of passion fruit shell base porous carbon materials；
Fig. 2 is the low temperature nitrogen adsorption isothermal curve of passion fruit shell base porous carbon materials；
Fig. 3 is the pore size distribution curve of passion fruit shell base porous carbon materials；
Fig. 4 is charge-discharge performance curve of the passion fruit shell base porous carbon materials in different current densities；
Fig. 5 is the electric capacity cyclic voltammogram of passion fruit shell base porous carbon materials；
Fig. 6 is passion fruit shell base porous carbon materials in 20 A g-1Loop test under current density；
Fig. 7 is the low temperature nitrogen adsorption isothermal curve of the passion fruit shell base porous carbon materials adulterated without additional nitrogen source；
Fig. 8 is the pore size distribution curve of the passion fruit shell base porous carbon materials adulterated without additional nitrogen source；
Fig. 9 is that the passion fruit shell base porous carbon materials adulterated without additional nitrogen source are bent in the charge-discharge performance of different current densities
Line.
Embodiment
The present invention is described in further detail by embodiment with reference to Figure of description to present invention, but is not pair
The limitation of the present invention.
Embodiment
Step 1）The low-temperature carbonization of passion fruit shell, passion fruit shell is cleaned, and cuts into the square particle of 1 cm, is dried
It is dry, 300 DEG C of low-temperature carbonization 2h in Muffle furnace are then placed on, product is filtered afterwards, wash, dry, ground, hundred are obtained fragrant
Shell base carbon material；
Step 2）The activation of passion fruit shell base carbon material, by gained sample and semicarbazides and KOH with 2.0：1.0：6.0 mass ratio
Mixing, is put into 50 ml deionized waters and is sufficiently stirred for, and it is calcined into 2h 800 DEG C under nitrogen protection after drying, N doping is obtained
Modified passion fruit shell base carbon material；
Step 3）The post processing of nitrogen-doped modified passion fruit shell base carbon material, above-mentioned product is soaked with 1M HCl solutions, and
Be washed with deionized, suction filtration to neutrality, after drying grind, obtain passion fruit shell base porous carbon materials.
By the scanned testing electronic microscope of passion fruit shell base porous carbon materials prepared in embodiment, as a result such as Fig. 1 institutes
Show, the carbon material shows cellular loose structure.
The passion fruit shell base porous carbon materials prepared in embodiment are tested through adsorption isothermal curve and pore-size distribution, as a result
As shown in Figures 2 and 3, as a result show, it has higher specific surface area, reaches 2603 m2 g-1, substantial amounts of micropore and appropriate
Mesoporous, average pore size is 1.92 nm, and pore volume is 1.25cm3g-1。
Using the passion fruit shell base porous carbon materials prepared in embodiment as electrode material for super capacitor apply when, permanent electricity
Charge-discharge test result is flowed as shown in figure 4, when current density is 0.5 A g-1When, specific capacitance value is up to 347 F g-1。
Using the passion fruit shell base porous carbon materials prepared in embodiment as electrode material for super capacitor apply when, circulation
Volt-ampere test result is as shown in figure 5, under different sweep speeds, and cyclic voltammetry curve keeps good and is similar to rectangle shape
Shape, shows there is the performance of good electric double layer capacitance.
Using the passion fruit shell base porous carbon materials prepared in embodiment as during the application of electrode material for super capacitor, survey
Test result is as shown in fig. 6, in 20 A g-1Under high current density, specific capacitance value is up to 252 F g-1, than electricity after being circulated at 10000 times
Holding conservation rate still has 88 %.
In order to contrast influence of the addition nitrogen source semicarbazides to carbon material structure and performance, further synthesis is mixed without additional nitrogen source
Miscellaneous passion fruit shell base porous carbon materials, the specific steps of its preparation method if not otherwise specified the step of with passion fruit shell Quito
The preparation method of hole carbon material is identical.
Difference is：Step（2）In without semicarbazides, only by gained sample and KOH with 1.0：2.0 mass ratio
Mixing, finally gives the passion fruit shell base porous carbon materials adulterated without additional nitrogen source.
To be prepared in embodiment the passion fruit shell base porous carbon materials that are adulterated without additional nitrogen source through adsorption isothermal curve and
Pore-size distribution is tested, as shown in FIG. 7 and 8, is had without the passion fruit shell based cellular structures carbon material that additional nitrogen source is adulterated wider
Pore-size distribution, low specific surface area are smaller, are 1505 m2 g-1It is 0.73cm with less pore volume3g-1。
It regard the passion fruit shell base porous carbon materials adulterated without additional nitrogen source prepared in embodiment as super capacitor electrode
During the application of pole material, constant current charge-discharge test result is as shown in figure 9, when current density is 0.5 A g-1When, specific capacitance value
For 261 F g-1。
In summary analyze, the passion fruit shell base porous carbon materials specific surface area and pore volume obtained after the addition of semicarbazides is equal
Increase, pore-size distribution are homogeneous, further enhancing its performance of the supercapacitor, and its specific capacity increases, followed under high current density
Ring performance is stable.
Claims (8)
1. a kind of passion fruit shell base porous carbon materials, it is characterised in that：By passion fruit shell handled through low-temperature carbonization after with nitrogen
Compound is mixed, and is then prepared from using alkali inorganic substance calcining and activating.
2. passion fruit shell base porous carbon materials according to claim 1, it is characterised in that：Specific surface area scope be 1500 ~
2603 m2 g-1, pore-size distribution is homogeneous, is distributed in the range of 1.80 ~ 2.40 nm.
3. the preparation method of passion fruit shell base porous carbon materials according to claim 1, it is characterised in that methods described includes
Following steps：
Step 1）The low-temperature carbonization of passion fruit shell, passion fruit shell is cleaned, block, drying is cut into, is placed in Muffle furnace in certain bar
Low-temperature carbonization under part, carbonized product is filtered, wash, dry, ground, and obtains passion fruit shell base carbon material；
Step 2）The activation of passion fruit shell base carbon material, by step 1）Gained passion fruit shell base carbon material and nitrogen-containing compound and alkali
Property inorganic matter by certain mass than mixing, in deionized water soak after, put into after drying in tube furnace nitrogen atmosphere protect
Under, nitrogen-doped modified passion fruit shell base carbon material is obtained with certain condition calcining and activating；
Step 3）The post processing of passion fruit shell base carbon material, above-mentioned product is soaked with hydrochloric acid solution, by washing, filtering, is dried
Dry, grinding obtains passion fruit shell base porous carbon materials.
4. preparation method according to claim 3, it is characterised in that：The step 1）In passion fruit shell low-temperature carbonization
Condition is is placed in Muffle furnace, at a temperature of 300 ~ 450 DEG C, 1 ~ 3h of low-temperature carbonization.
5. preparation method according to claim 3, it is characterised in that：The step 2）In nitrogen-containing compound be amino
Urea, urea or guanidine carbonate, the step 2）In alkali inorganic substance be potassium hydroxide, sodium hydroxide, potassium carbonate or zinc chloride.
6. preparation method according to claim 3, it is characterised in that：The step 2）In passion fruit shell base carbon material with
The mass ratio of nitrogen-containing compound and alkali inorganic substance is 1.0：（0.5~4.0）：（1.5~6.0）.
7. preparation method according to claim 3, it is characterised in that：The step 2）In calcining and activating condition for live
It is 600 ~ 900 DEG C to change temperature, and soak time is 1 ~ 6 h.
8. passion fruit shell base porous carbon materials are as the application of electrode material for super capacitor according to claim 1, it is special
Levy and be：When current density is 0.5 A g-1When, specific capacitance value scope is in 261 ~ 347F g-1。
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| CN108054023A (en) * | 2017-12-15 | 2018-05-18 | 桂林电子科技大学 | A kind of nitrating porous carbon materials based on phenolic resin and its preparation method and application |
| CN108455600A (en) * | 2018-03-07 | 2018-08-28 | 郑州大学 | A kind of preparation method of biomass graded porous carbon materials |
| CN108753905A (en) * | 2018-06-27 | 2018-11-06 | 湖南大学 | A kind of application of porous carbon materials |
| CN109319778A (en) * | 2018-09-25 | 2019-02-12 | 桂林电子科技大学 | A kind of preparation method and application of N doping pine nut shell base porous carbon materials |
| CN109592665A (en) * | 2019-01-21 | 2019-04-09 | 兖矿集团有限公司 | A kind of preparation method of nanoporous carbon materials |
| CN109761235A (en) * | 2018-11-01 | 2019-05-17 | 南昌航空大学 | A kind of synthetic method of biological material walnut shell carbon material nitrating and its application in terms of anode of microbial fuel cell |
| CN110124721A (en) * | 2019-05-24 | 2019-08-16 | 桂林电子科技大学 | A kind of nitrogen-doped porous carbon material and its preparation method and application of load C oB nanoparticle |
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| CN108054023A (en) * | 2017-12-15 | 2018-05-18 | 桂林电子科技大学 | A kind of nitrating porous carbon materials based on phenolic resin and its preparation method and application |
| CN108455600A (en) * | 2018-03-07 | 2018-08-28 | 郑州大学 | A kind of preparation method of biomass graded porous carbon materials |
| CN108455600B (en) * | 2018-03-07 | 2021-04-27 | 郑州大学 | Preparation method of biomass graded porous carbon material |
| CN108753905A (en) * | 2018-06-27 | 2018-11-06 | 湖南大学 | A kind of application of porous carbon materials |
| CN109319778A (en) * | 2018-09-25 | 2019-02-12 | 桂林电子科技大学 | A kind of preparation method and application of N doping pine nut shell base porous carbon materials |
| CN109761235A (en) * | 2018-11-01 | 2019-05-17 | 南昌航空大学 | A kind of synthetic method of biological material walnut shell carbon material nitrating and its application in terms of anode of microbial fuel cell |
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| CN109592665A (en) * | 2019-01-21 | 2019-04-09 | 兖矿集团有限公司 | A kind of preparation method of nanoporous carbon materials |
| CN110124721A (en) * | 2019-05-24 | 2019-08-16 | 桂林电子科技大学 | A kind of nitrogen-doped porous carbon material and its preparation method and application of load C oB nanoparticle |
| CN110124721B (en) * | 2019-05-24 | 2022-10-04 | 桂林电子科技大学 | CoB nanoparticle-loaded nitrogen-doped porous carbon material and preparation method and application thereof |
| CN110277249A (en) * | 2019-07-01 | 2019-09-24 | 湖南城市学院 | A method of high-performance super capacitor negative electrode material is prepared using passion fruit shell |
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| CN115140735A (en) * | 2022-05-27 | 2022-10-04 | 桂林理工大学 | Preparation method and application of passion fruit peel-based activated carbon |
| CN115414913A (en) * | 2022-09-22 | 2022-12-02 | 中国热带农业科学院分析测试中心 | Biochar prepared from passion fruit peel and preparation method thereof |
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Application publication date: 20171103 |