CN109904007A - A kind of preparation method of spongy nitrogen sulphur codope porous carbon electrode material - Google Patents
A kind of preparation method of spongy nitrogen sulphur codope porous carbon electrode material Download PDFInfo
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- CN109904007A CN109904007A CN201910116285.8A CN201910116285A CN109904007A CN 109904007 A CN109904007 A CN 109904007A CN 201910116285 A CN201910116285 A CN 201910116285A CN 109904007 A CN109904007 A CN 109904007A
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- sulphur codope
- nitrogen sulphur
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Abstract
The present invention provides a kind of preparation methods of spongy nitrogen sulphur codope porous carbon electrode material characterized by comprising step 1: pomelo peel stripping and slicing is washed, it is dry, and grind into powder；Step 2: by pomelo peel powder and ammonium persulfate mixed grinding to fully dispersed；Step 3: the resulting pre- carburizing reagent of mixture high temperature of step 2 is obtained into nitrogen sulphur codope carbon matrix precursor；Step 4: resulting nitrogen sulphur codope carbon matrix precursor being mixed into dispersion juxtaposition with KOH and is dried in vacuo in a vacuum drying oven；Step 5: the product high-temperature roasting after drying being handled to obtain spongy nitrogen sulphur codope porous carbon electrode material.Preparation method of the invention is simple, easy to operate, and raw material is cheap and easy to get.
Description
Technical field
Present invention relates particularly to field of material technology, more particularly to a kind of spongy nitrogen sulphur codope porous carbon electrodes material
The preparation method of material.
Background technique
The energy is always an important problem for the mankind.Ever-increasing demographic and economic development, improves
The consumption of fossil fuel leads to a large amount of greenhouse gas emission, climate change, causes environmental problem.Production and storage inhomogeneity
The alternative of type energy is becoming the mission that the mankind urgently complete.Renewable energy, because of its low cost and environmental-friendly spy
Property is one of the mode of most attraction.Critical issue in a manner of sustainable using renewable energy is how effectively to store up
Deposit energy and meet demand.Therefore, the importance of energy storage equipment is approved recently.Supercapacitor is also electricity
Chemical capacitor, as a kind of emerging energy storage device, due to charge-discharge velocity is fast, have extended cycle life, power density is high the features such as,
It is widely used in the fields such as communications and transportation, industrial production.In the capacitor, electrode material is crucial, it is resolved that the master of capacitor
Want performance indicator.
Porous carbon materials are due to large specific surface area, pore structure prosperity, acid and alkali-resistance, corrosion-resistant, excellent conductivity, being easy to
Properties and the features such as design and aperture are adjustable, are widely used as the electrode material of novel energy storage apparatus, industrially show
Huge application potential, and by regulating and controlling its composed structure to obtain more preferably performance and realize that the control of preparation cost is always
The emphasis of research.Two-dimentional porous carbon materials are capable of providing shorter electrolyte diffusion channel and faster electronic transmission process, because
This shows the theory of excellent chemical property in recent years in energy conversion and storage device and shows with experimental study, and two
Element codope can make the chemical property of two-dimentional porous carbon materials be improved significantly therefore, codope porous carbon materials
It is prepared into current one of research hotspot.
Summary of the invention
The object of the present invention is to provide a kind of preparations of the spongy nitrogen sulphur codope porous carbon electrode material of simple possible
Method, to solve preparation process the high requirements on the equipment, the reaction condition of existing spongy nitrogen sulphur codope porous carbon electrode material
The technical problems such as harshness.
In order to achieve the above object, the present invention provides a kind of preparations of spongy nitrogen sulphur codope porous carbon electrode material
Method characterized by comprising
Step 1: pomelo peel stripping and slicing is washed, it is dry, and grind into powder；
Step 2: by pomelo peel powder and ammonium persulfate mixed grinding to fully dispersed；
Step 3: the resulting pre- carburizing reagent of mixture high temperature of step 2 is obtained into nitrogen sulphur codope carbon matrix precursor；
Step 4: resulting nitrogen sulphur codope carbon matrix precursor is mixed with KOH to dispersion juxtaposition, and vacuum is done in a vacuum drying oven
It is dry；
Step 5: the product high-temperature roasting after drying being handled to obtain spongy nitrogen sulphur codope porous carbon electrode material.
Preferably, the preparation method of the spongy nitrogen sulphur codope porous carbon electrode material further include:
Step 6: mixed with acetylene black and PTFE emulsion after obtained spongy nitrogen sulphur codope porous carbon abrasive lapping
It closes, ultrasonic disperse obtains electrode material.
Preferably, the drying temperature in the step 1 be 100~200 DEG C, drying time be 12~for 24 hours.
Preferably, the mass ratio of pomelo peel powder and ammonium persulfate is 1:1~4 in the step 2.
Preferably, reaction temperature is 400~800 DEG C in the step 3, and the reaction time is 2~8h.
Preferably, the mass ratio of nitrogen sulphur codope carbon matrix precursor and KOH obtained in the step 4 are 1:1~4, are done
Dry temperature be 60~100 DEG C, drying time be 12~for 24 hours.
Preferably, maturing temperature is 400~1000 DEG C in the step 5, and calcining time is 2~8h.
Preferably, it roasts in the step 5 and carries out under nitrogen atmosphere.
Preferably, spongy nitrogen sulphur codope porous carbon materials in the step 6, acetylene black and PTFE emulsion ratio
For 8mg:1mg:100 μ l, the solid content of PTFE emulsion is 5%-20%.
The spongy nitrogen sulphur codope carbon material that the present invention obtains is with KOH solution or H2SO4Solution is as electrolyte, selection
Three-electrode system measures its chemical property, and three-electrode system reference electrode can be Ag/AgCl reference electrode, saturation HgCl2
Reference electrode.
Compared with existing scheme, the beneficial effects of the present invention are: preparation process of the present invention is simple, only with two step Gao Wenre
Solution, source is biomass castoff, has the characteristics that environmentally friendly, prepared spongy nitrogen sulphur codope porous carbon electrodes material
Expect that size is more uniform, simple to operate, economic and practical is strong, and raw material is relatively inexpensive to be easy to get, and production cost is low, has wide
Application prospect and market potential.
Detailed description of the invention
Fig. 1 is the SEM figure of spongy nitrogen sulphur codope porous carbon electrode material prepared by embodiment 1.
Fig. 2 is the SEM figure of spongy nitrogen sulphur codope porous carbon electrode material prepared by embodiment 2.
Fig. 3 is the TEM figure of spongy nitrogen sulphur codope porous carbon electrode material prepared by embodiment 3.
Fig. 4 is the TEM figure of spongy nitrogen sulphur codope porous carbon electrode material prepared by embodiment 4.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
A kind of preparation method of spongy nitrogen sulphur codope porous carbon electrode material, specific steps are as follows:
(1) fresh grapefruit skin is cut into small pieces, is washed with deionized, and dried for 24 hours at 100 DEG C, grind into powder；
(2) by 1g pomelo peel powder and 1g ammonium persulfate mixed grinding until fully dispersed；
(3) by resulting mixture, the pre- carburizing reagent 2h of high temperature obtains nitrogen sulphur codope carbon matrix precursor at 500 DEG C；
(4) nitrogen sulphur codope carbon matrix precursor obtained by 0.5g and 0.5g KOH are dissolved in 5ml deionized water and are sufficiently mixed point
Scattered juxtaposition is dried in vacuo 12h at 60 DEG C in a vacuum drying oven；
(5) finally by dried transferred product to tube furnace, under nitrogen atmosphere, with 5 degrees Celsius of heating per minute
Rate is warming up to 600 DEG C of high-temperature roasting 2h, obtains spongy nitrogen sulphur codope porous carbon electrode material, from scanning electron microscope (SEM) photograph (figure
1) it can be seen that material is spongelike structure in.
(6) after obtained spongy nitrogen sulphur codope carbon material being ground to 100 mesh, electronic balance precise sample is used
Product 8mg, is added in the centrifuge tube of 2ml, and 1mg acetylene black and 100 μ l solid contents are added and mix for 10% PTFE emulsion, then
It is put into ultrasonic cleaning machine and carries out ultrasonic disperse, obtain required electrode material, by electrode material coated in nickel foam, apply
Thickness is about 0.1~0.5 μm.
Spongy nitrogen sulphur codope carbon material electrochemical property test: electrochemical workstation is used, in three-electrode system
Electrochemical property test is carried out to the spongy nitrogen sulphur codope carbon electrode of preparation.Using the KOH solution of 6M as electrolyte, work
Electrode is spongy nitrogen sulphur codope carbon electrode, and auxiliary electrode is platinized platinum, and reference electrode is Ag/AgCl electrode.Work as current density
When for 0.5A/g, the specific capacitance of material is 335F/g.
Embodiment 2
A kind of preparation method of spongy nitrogen sulphur codope porous carbon electrode material, specific steps are as follows:
(1) fresh grapefruit skin is cut into small pieces, is washed with deionized, and the dry 12h at 120 DEG C, grind into powder；
(2) by 1g pomelo peel powder and 2g ammonium persulfate mixed grinding until fully dispersed；
(3) by resulting mixture, the pre- carburizing reagent 2h of high temperature obtains nitrogen sulphur codope carbon matrix precursor at 400 DEG C；
(4) nitrogen sulphur codope carbon matrix precursor obtained by 0.5g and 2g KOH are dissolved in 5ml deionized water and are sufficiently mixed dispersion
Juxtaposition is dried in vacuo 12h at 100 DEG C in a vacuum drying oven；
(5) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, with 5 degrees Celsius of heating per minute
Rate is warming up to 700 DEG C of high-temperature roasting 2h, obtains spongy nitrogen sulphur codope porous carbon electrode material, from scanning electron microscope (SEM) photograph (figure
2) it can be seen that material is spongelike structure in.
(6) after obtained spongy nitrogen sulphur codope carbon material being ground to 100 mesh, electronic balance precise sample is used
Product 8mg, is added in the centrifuge tube of 2ml, and 1mg acetylene black and 100 μ l solid contents are added and mix for 15% PTFE emulsion, then
It is put into ultrasonic cleaning machine and carries out ultrasonic disperse, obtain required electrode material.By electrode material coated in nickel foam, apply
Thickness is about 0.1~0.5 μm.
(7) spongy nitrogen sulphur codope carbon material electrochemical property test: electrochemical workstation is used, in three-electrode system
In electrochemical property test is carried out to the spongy nitrogen sulphur codope carbon electrode of preparation.Using the KOH solution of 6M as electrolyte, work
Making electrode is spongy nitrogen sulphur codope carbon electrode, and auxiliary electrode is platinized platinum, and reference electrode is Ag/AgCl electrode.When electric current is close
When degree is 0.5A/g, the specific capacitance of material is 323F/g.
Embodiment 3
A kind of preparation method of spongy nitrogen sulphur codope porous carbon electrode material, specific steps are as follows:
(1) fresh grapefruit skin is cut into small pieces, is washed with deionized, and the dry 12h at 150 DEG C, grind into powder；
(2) by 1g pomelo peel powder and 3g ammonium persulfate mixed grinding until fully dispersed；
(3) by resulting mixture, the pre- carburizing reagent 4h of high temperature obtains nitrogen sulphur codope carbon matrix precursor at 600 DEG C；
(4) nitrogen sulphur codope carbon matrix precursor obtained by 0.5g and 1g KOH are dissolved in 5ml deionized water and are sufficiently mixed dispersion
Juxtaposition is dried in vacuo for 24 hours at 80 DEG C in a vacuum drying oven；
(5) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, with 5 degrees Celsius of heating per minute
Rate is warming up to 800 DEG C of high-temperature roasting 4h, obtains spongy nitrogen sulphur codope porous carbon electrode material.From transmission electron microscope picture (figure
3) obvious it can be seen that material is spongelike structure, rough surface in.
(6) after obtained spongy nitrogen sulphur codope carbon material being ground to 100 mesh, electronic balance precise sample is used
Product 8mg, is added in the centrifuge tube of 2ml, and 1mg acetylene black and 100 μ l solid contents are added and mix for 5% PTFE emulsion, then
It is put into ultrasonic cleaning machine and carries out ultrasonic disperse, obtain required electrode material.
(7) by electrode material coated in nickel foam, applied thickness is about 0.1~0.5 μm.
(8) spongy nitrogen sulphur codope carbon material electrochemical property test: electrochemical workstation is used, in three-electrode system
In electrochemical property test is carried out to the spongy nitrogen sulphur codope carbon electrode of preparation.With the H of 1M2SO4Solution as electrolyte,
Working electrode is spongy nitrogen sulphur codope carbon electrode, and auxiliary electrode is platinized platinum, and reference electrode is Ag/AgCl electrode.Work as electric current
When density is 0.5A/g, the specific capacitance of material is 301F/g.
Embodiment 4
A kind of preparation method of spongy nitrogen sulphur codope porous carbon electrode material, specific steps are as follows:
(1) fresh grapefruit skin is cut into small pieces, is washed with deionized, and dried for 24 hours at 200 DEG C, grind into powder；
(2) by 1g pomelo peel powder and 4g ammonium persulfate mixed grinding until fully dispersed；
(3) by resulting mixture, the pre- carburizing reagent 2h of high temperature obtains nitrogen sulphur codope carbon matrix precursor at 800 DEG C；
(4) nitrogen sulphur codope carbon matrix precursor obtained by 0.5g and 1g KOH are dissolved in 5ml deionized water and are sufficiently mixed dispersion
Juxtaposition is dried in vacuo for 24 hours at 60 DEG C in a vacuum drying oven；
(5) dried sample is finally transferred to tube furnace, under nitrogen atmosphere, with 5 degrees Celsius of heating per minute
Rate is warming up to 1000 DEG C of high-temperature roasting 2h, obtains spongy nitrogen sulphur codope porous carbon electrode material.From transmission electron microscope picture (figure
4) obvious it can be seen that material is spongelike structure, rough surface in.
(6) after obtained spongy nitrogen sulphur codope carbon material being ground to 100 mesh, electronic balance precise sample is used
Product 8mg, is added in the centrifuge tube of 2ml, and 1mg acetylene black and 100 μ l solid contents are added and mix for 10% PTFE emulsion, then
It is put into ultrasonic cleaning machine and carries out ultrasonic disperse, obtain required electrode material.
(7) by electrode material coated in nickel foam, applied thickness is about 0.1~0.5 μm.
(8) spongy nitrogen sulphur codope carbon material electrochemical property test: electrochemical workstation is used, in three-electrode system
In electrochemical property test is carried out to the spongy nitrogen sulphur codope carbon electrode of preparation.With the H of 1M2SO4Solution as electrolyte,
Working electrode is spongy nitrogen sulphur codope carbon electrode, and auxiliary electrode is platinized platinum, and reference electrode is Ag/AgCl electrode.Work as electric current
When density is 0.5A/g, the specific capacitance of material is 323F/g.
Compared with conventional porous carbon electrode material have more regular structure, pattern from SEM figure it can be seen that.Sea
Continuous shape nitrogen sulphur codope porous carbon electrode material size is more uniform, and simple to operate, economic and practical is strong, and raw material sources are wide
General, production cost is low, has broad application prospects and market potential.
Above content is only the basic explanation under present inventive concept, and that technical solution according to the present invention is done is any etc.
Effect transformation, is within the scope of protection of the invention.
Claims (9)
1. a kind of preparation method of spongy nitrogen sulphur codope porous carbon electrode material characterized by comprising
Step 1: pomelo peel stripping and slicing is washed, it is dry, and grind into powder；
Step 2: by pomelo peel powder and ammonium persulfate mixed grinding to fully dispersed；
Step 3: the resulting pre- carburizing reagent of mixture high temperature of step 2 is obtained into nitrogen sulphur codope carbon matrix precursor；
Step 4: resulting nitrogen sulphur codope carbon matrix precursor being mixed into dispersion juxtaposition with KOH and is dried in vacuo in a vacuum drying oven；
Step 5: the product high-temperature roasting after drying being handled to obtain spongy nitrogen sulphur codope porous carbon electrode material.
2. the preparation method of spongy nitrogen sulphur codope porous carbon electrode material as described in claim 1, which is characterized in that also
Include: step 6: after obtained spongy nitrogen sulphur codope porous carbon abrasive lapping, being mixed with acetylene black and PTFE emulsion, is surpassed
Sound dispersion, obtains electrode material.
3. the preparation method of spongy nitrogen sulphur codope porous carbon electrode material as claimed in claim 2, which is characterized in that institute
The ratio of spongy nitrogen sulphur codope porous carbon materials, acetylene black and PTFE emulsion is 8mg:1mg:100 μ l in the step 6 stated,
The solid content of PTFE emulsion is 5%-20%.
4. the preparation method of spongy nitrogen sulphur codope porous carbon electrode material as described in claim 1, which is characterized in that institute
Drying temperature in the step 1 stated is 100~200 DEG C, drying time is 12~for 24 hours.
5. the preparation method of spongy nitrogen sulphur codope porous carbon electrode material as described in claim 1, which is characterized in that institute
The mass ratio of pomelo peel powder and ammonium persulfate is 1:1~4 in the step 2 stated.
6. the preparation method of spongy nitrogen sulphur codope porous carbon electrode material as described in claim 1, which is characterized in that institute
Reaction temperature is 400~800 DEG C in the step 3 stated, and the reaction time is 2~8h.
7. the preparation method of spongy nitrogen sulphur codope porous carbon electrode material as described in claim 1, which is characterized in that institute
The mass ratio of nitrogen sulphur codope carbon matrix precursor and KOH obtained in the step 4 stated are 1:1~4, and drying temperature is 60~100 DEG C,
Drying time be 12~for 24 hours.
8. the preparation method of spongy nitrogen sulphur codope porous carbon electrode material as described in claim 1, which is characterized in that institute
Maturing temperature is 400~1000 DEG C in the step 5 stated, and calcining time is 2~8h.
9. the preparation method of spongy nitrogen sulphur codope porous carbon electrode material as described in claim 1, which is characterized in that institute
It roasts in the step 5 stated and carries out under nitrogen atmosphere.
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| CN111234848A (en) * | 2020-01-14 | 2020-06-05 | 常州工学院 | Method for co-producing phenol-rich bio-oil and super capacitor material by biomass pyrolysis |
| CN111268675A (en) * | 2020-02-28 | 2020-06-12 | 上海应用技术大学 | Method for preparing nitrogen-phosphorus co-doped carbon material by taking durian peel as raw material |
| CN112194128A (en) * | 2020-10-22 | 2021-01-08 | 中国科学院山西煤炭化学研究所 | Preparation method and application of active carbon material prepared by double doping of nitrogen and sulfur in furfural residues |
| CN115007193A (en) * | 2022-07-18 | 2022-09-06 | 南华大学 | Carbon-based catalyst, preparation method and application thereof, and activated persulfate continuous sewage purification system |
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