CN110085438A - A kind of preparation method of nitrogen oxygen codope porous carbon - Google Patents
A kind of preparation method of nitrogen oxygen codope porous carbon Download PDFInfo
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- CN110085438A CN110085438A CN201910322860.XA CN201910322860A CN110085438A CN 110085438 A CN110085438 A CN 110085438A CN 201910322860 A CN201910322860 A CN 201910322860A CN 110085438 A CN110085438 A CN 110085438A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention provides a kind of preparation methods of nitrogen oxygen codope porous carbon, belong to materials chemistry technical field of inorganic non-metal material preparation.The material is made by following methods: this method is using cheap diatomite as foraminous die plate, using dopamine as raw material, alkaline solution is adsorbed after in-situ polymerization, the doping for realizing carbonization, pore-forming and nitrogen simultaneously by a step high-temperature annealing process reuses while strong base solution removes template and adulterates oxygen element.This method is low in cost, easy to operate, with short production cycle, is easy to realize industrial production, and resulting materials not only have a large amount of holes but also succeed nitrogen doped and oxygen element, can be used as electrode material for super capacitor and catalysis material etc..
Description
Technical field
The invention belongs to technical field of material chemistry, are related to a kind of inorganic non-metallic material, more specifically to a kind of nitrogen oxygen
The preparation method of codope porous carbon.
Background technique
With scientific and technological progress, requirement of the mankind to material property increasingly increases, and conventional material has been unable to satisfy higher need
It asks, thus the material with special appearance and performance gradually obtains the attention of scientific circles.
Porous carbon materials due to easily being modified with high-specific surface area, surface, it is good conductive and heating conduction, high mechanical steady
Qualitative, high temperature resistant, acid and alkali-resistance and it is low in cost the features such as and paid close attention to by researchers at home and abroad, and then be widely used in
The fields such as absorption, separation, purification, catalysis, sensing, medicine and energy stores.
Commercial porous active carbon material has excellent follow as the electrode material of energy storage device supercapacitor
Ring stability, however, absorbent charcoal material has a large amount of micropore, ion is difficult to spread absorption, leads to the practical than electricity of the material
Hold that lower and high rate performance is poor, limits the further development of supercapacitor to a certain extent.In order to improve carbon material
Chemical property, one side researcher by design meso-hole structure improve carbon material effective ratio area, on the other hand draw
Enter the fake capacitance that hetero atom (such as nitrogen-atoms, oxygen atom) doping improves carbon material.It is counterfeit that research finds that nitrogen-atoms can not only play
Capacitor increases the capacitive property of material, and there are nitrogen-atoms additional lone pair electrons can enhance electron transport property and chemistry instead
Activity is answered, in addition, the introducing of nitrogen-atoms can increase the wellability of material in the electrolytic solution, and then the whole electrification for improving material
Learn performance.Researcher also found that a variety of hetero atom codopes are able to achieve synergistic effect, further promote the capacitive property of carbon material.
However, the now widely used method for preparing azepine porous carbon with silicon-based mesoporous material (SBA) for template, template can not return
Receive, cost costly, complex process and time-consuming.Therefore, development cost cheap method prepares a variety of Heteroatom dopings
Porous carbon is necessary and significant.
Summary of the invention
In view of the deficienciess of the prior art, the type of horn of plenty material, solve customary preparation methods complex process and at
This higher problem.The present invention provides a kind of preparation methods of nitrogen oxygen codope porous carbon.This method using diatomite as template,
Dopamine is raw material, prepares a kind of nitrogen oxygen codope porous carbon materials.This method template is easy to get, is low in cost, and product can
As electrode material for super capacitor and catalysis material etc..
To achieve the above object, the technical solution adopted in the present invention is as follows:
A kind of preparation method of nitrogen oxygen codope porous carbon, it includes following steps:
A. diatomite/poly-dopamine composite material preparation: diatomite and dopamine are added into weakly alkaline solution, often
It is stirred to react a period of time under temperature, material filter cake is obtained by filtration；
B. it washs: the material filter cake being obtained by filtration directly is washed with deionized water, or directly with deionized water after drying
Washing；
C. it impregnates: the composite material filter cake that step B is obtained is added into alkaline solution, when stirring impregnates one section under room temperature
Between, material filter cake is obtained by filtration；
D. be carbonized: by the material filter cake being obtained by filtration, high temperature cabonization for a period of time, is cooled to room temperature under an inert atmosphere, is obtained
To diatomite/azepine carbon composite；
E. removing template: obtained diatomite/azepine carbon composite is added into alkaline solution, hydro-thermal under certain temperature
Reaction removes template and realizes that oxygen atom adulterates simultaneously, is cooled to room temperature, material filter cake is obtained by filtration；
F. it washs: the material filter cake being obtained by filtration directly is washed with deionized water；
G. it dries: the washed material filtration cakes torrefaction of deionized water is obtained into nitrogen oxygen codope porous carbon materials.
The additive amount of diatomite is 1.0-200.0g/L in the step A, and the additive amount of dopamine is 2.0-
400.0g/L, weakly alkaline solution concentration are 0.001-1.0mol/L, and the reaction time is 6.0-48.0 hours.
The weakly alkaline solution refers to tris solution.
Washing refers to that the composite material filter cake being obtained by filtration adds deionized water to filter elution at room temperature in the step B,
Or deionized water is added to filter elution at room temperature after 55.0-85.0 DEG C of the material filter cake being obtained by filtration drying.
The step C neutral and alkali solution concentration is 1.0-12.0mol/L, and soaking time is 0.05-48.0 hours.
The alkaline solution refers to potassium hydroxide solution.
Inert atmosphere is preferably argon atmosphere in the step D, and carburizing temperature is 400.0-1200.0 DEG C, and the time is
1.0-24.0 hour.
The step E neutral and alkali solution concentration is 5.0-15.0mol/L, and reaction temperature is 100.0-300.0 DEG C, reaction
Time is 5.0-50.0 hours.
The alkaline solution refers to sodium hydroxide or potassium hydroxide solution.
Washing refers to that the material filter cake being obtained by filtration adds deionized water to filter elution at room temperature in the step F；
In the step G it is dry refer to washed material filter cake through 55.0-85.0 DEG C drying 5.0-10.0 hours,
Or freeze-drying 10-48.0 hours of -50.0-90.0 DEG C of warp obtains nitrogen oxygen codope porous carbon materials.
A kind of preparation method of nitrogen oxygen codope porous carbon materials of the invention, using diatomite cheap and easy to get as template,
Dopamine is raw material, and the processes such as aggregated, carbonization, removing template obtain nitrogen oxygen codope porous carbon materials.Compared with prior art,
Method provided by the invention is low in cost, easy to operate, with short production cycle, is easy to realize industrial production, and resulting nitrogen oxygen
Codope porous carbon materials are in addition to multi-stage pore structure abundant, being also successfully realized being co-doped with for nitrogen and oxygen element
It is miscellaneous.
Detailed description of the invention
In order to state the technical solution of the inventive embodiments more full and accurately, below to attached drawing used in embodiment description
It is briefly described.Obviously, the attached drawing in being described below is only some embodiments of the present invention, for those of ordinary skill in the art
For, under the premise of not being put to creative work, other attached drawings can be also obtained according to such attached drawing.
Fig. 1 is that the low power scanning electron microscope of the nitrogen oxygen codope porous carbon materials obtained in the embodiment of the present invention one is shone
Piece；
Fig. 2 is that the high power scanning electron microscope of the nitrogen oxygen codope porous carbon materials obtained in the embodiment of the present invention one is shone
Piece；
Fig. 3 is that the low power scanning electron microscope of the nitrogen oxygen codope porous carbon materials obtained in the embodiment of the present invention two is shone
Piece；
Fig. 4 is that the high power scanning electron microscope of the nitrogen oxygen codope porous carbon materials obtained in the embodiment of the present invention two is shone
Piece；
Fig. 5 is that the low power scanning electron microscope of the nitrogen oxygen codope porous carbon materials obtained in the embodiment of the present invention three is shone
Piece；
Fig. 6 is that the high power scanning electron microscope of the nitrogen oxygen codope porous carbon materials obtained in the embodiment of the present invention three is shone
Piece；
Fig. 7 is the X-ray photoelectron spectroscopic analysis of the nitrogen oxygen codope porous carbon materials obtained in the embodiment of the present invention one
Spectrogram；
Fig. 8 is the circulation volt that the nitrogen oxygen codope porous carbon materials obtained in the embodiment of the present invention one are used for supercapacitor
Antu；
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, those skilled in the art is made to more fully understand this
Invention, with reference to the accompanying drawing further elaborates embodiments of the present invention with embodiment.
Embodiment 1
(1) trishydroxymethylaminomethane of 0.121g is added in 150mL deionized water, to after completely dissolution with dense salt
The titration of the dilute hydrochloric acid of acid or any concentration adjusts pH to 8.5, and 1.0g diatomite and 2.5g DOPA are then added under stirring at normal temperature
Amine reacts 24.0 hours, and filtering, filter cake washs to obtain diatomite/poly-dopamine composite material with deionized water.
(2) diatomite/poly-dopamine composite material that step (1) obtains is added to 100.0mL concentration is 3.0mol/L
Potassium hydroxide solution in, under room temperature stirring impregnate 3.0 hours, material filter cake is obtained by filtration；
(3) the material filter cake for obtaining step (2) is carbonized 2.0 hours for 800.0 DEG C under an argon atmosphere, is cooled to room temperature,
Obtain diatomite/azepine carbon composite；
(4) diatomite/azepine carbon composite that step (3) obtains is added to 200.0mL concentration is 12.0 mol/L
Sodium hydroxide solution in, 180.0 DEG C are cooled to room temperature after hydro-thermal reaction 24.0 hours, filter, filter cake is directly with deionized water
Washing, -60.0 DEG C of warp of washed composite material filter cake freeze-dryings obtain nitrogen oxygen codope porous carbon materials in 24.0 hours.
Microscopic appearance and composition measurement are carried out to a kind of above-mentioned nitrogen oxygen codope porous carbon materials for being prepared, obtain as
Fig. 1 and electron scanning micrograph shown in Fig. 2, X-ray photoelectron spectroscopic analysis spectrogram as shown in Figure 7；To above-mentioned system
A kind of standby obtained nitrogen oxygen codope porous carbon materials carry out supercapacitor applications research, obtain circulation volt as shown in Figure 8
Antu.
Embodiment 2
(1) trishydroxymethylaminomethane of 1.21g is added in 200mL deionized water, to after completely dissolution with dense salt
The titration of the dilute hydrochloric acid of acid or any concentration adjusts pH to 8.2, and 2.0 g diatomite and 8.0g DOPA are then added under stirring at normal temperature
Amine reacts 12.0 hours, and filtering, filter cake washs to obtain diatomite/poly-dopamine composite material with deionized water.
(2) diatomite/poly-dopamine composite material that step (1) obtains is added to 200.0mL concentration is 6.0mol/L
Potassium hydroxide solution in, under room temperature stirring impregnate 0.5 hour, material filter cake is obtained by filtration；
(3) the material filter cake for obtaining step (2) is carbonized 3.0 hours for 700.0 DEG C under an argon atmosphere, is cooled to room temperature,
Obtain diatomite/azepine carbon composite；
(4) diatomite/azepine carbon composite that step (3) obtains is added to 500.0mL concentration is 15.0 mol/L
Sodium hydroxide solution in, 160.0 DEG C are cooled to room temperature after hydro-thermal reaction 48.0 hours, filter, filter cake is directly with deionized water
Washing, washed composite material filter cake dry 5.0 hours through 60 DEG C and obtain nitrogen oxygen codope porous carbon materials.
Microscopic appearance and composition measurement are carried out to a kind of above-mentioned nitrogen oxygen codope porous carbon materials material being prepared, obtained
To electron scanning micrograph as shown in Figure 3 and Figure 4, X-ray photoelectron spectroscopic analysis spectrogram similar to Figure 7 is right
A kind of above-mentioned nitrogen oxygen codope porous carbon materials being prepared carry out supercapacitor applications research, obtain similar to Figure 8
Cyclic voltammogram.
Embodiment 3
(1) trishydroxymethylaminomethane of 3.0g is added in 300mL deionized water, to use concentrated hydrochloric acid after completely dissolution
Or the dilute hydrochloric acid titration of any concentration adjusts pH to 8.7, and 4.0 g diatomite and 10.0g DOPA are then added under stirring at normal temperature
Amine reacts 48.0 hours, and filtering, filter cake washs to obtain diatomite/poly-dopamine composite material with deionized water.
(2) diatomite/poly-dopamine composite material that step (1) obtains is added to 150.0mL concentration is 9.0mol/L
Potassium hydroxide solution in, under room temperature stirring impregnate 24.0 hours, material filter cake is obtained by filtration；
(3) the material filter cake for obtaining step (2) is carbonized 1.0 hours for 900.0 DEG C under an argon atmosphere, is cooled to room temperature,
Obtain diatomite/azepine carbon composite；
(4) diatomite/azepine carbon composite that step (3) obtains is added to 800.0mL concentration is 10.0 mol/L
Sodium hydroxide solution in, 220.0 DEG C are cooled to room temperature after hydro-thermal reaction 12.0 hours, filter, filter cake is directly with deionized water
Washing, -80.0 DEG C of warp of washed composite material filter cake freeze-dryings obtain nitrogen oxygen codope porous carbon materials in 10.0 hours.
Microscopic appearance and composition measurement are carried out to a kind of above-mentioned nitrogen oxygen codope porous carbon materials for being prepared, obtain as
Fig. 5 and electron scanning micrograph shown in fig. 6, X-ray photoelectron spectroscopic analysis spectrogram similar to Figure 7, to above-mentioned
A kind of nitrogen oxygen codope porous carbon materials being prepared carry out supercapacitor applications research, obtain similar to Figure 8 follow
Ring voltammogram.
Embodiment described above is only that the present invention is described further, however the present invention is not limited to this, all not
Any modification, equivalent replacement or the improvement etc. made in the case where being detached from core of the present invention, should be included in protection of the invention
In range.
Claims (10)
1. a kind of preparation method of nitrogen oxygen codope porous carbon, which is characterized in that comprise the steps of:
A. diatomite/poly-dopamine composite material preparation: diatomite and dopamine are added into weakly alkaline solution, under room temperature
It is stirred to react a period of time, material filter cake is obtained by filtration；
B. it washs: the material filter cake being obtained by filtration directly is washed with deionized water, or directly washed after drying with deionized water；
C. it impregnating: the composite material filter cake that step B is obtained is added into alkaline solution, stirring is soaked for a period of time under room temperature,
Material filter cake is obtained by filtration；
D. be carbonized: by the material filter cake being obtained by filtration, high temperature cabonization for a period of time, is cooled to room temperature under an inert atmosphere, obtains silicon
Diatomaceous earth/azepine carbon composite；
E. removing template: obtained diatomite/azepine carbon composite is added into alkaline solution, hydro-thermal reaction under certain temperature
It removes template and realizes that oxygen atom adulterates, be cooled to room temperature, material filter cake is obtained by filtration；
F. it washs: the material filter cake being obtained by filtration directly is washed with deionized water；
G. it dries: the washed material filtration cakes torrefaction of deionized water is obtained into nitrogen oxygen codope porous carbon materials.
2. a kind of preparation method of nitrogen oxygen codope porous carbon according to claim 1, which is characterized in that in step A, silicon
For diatomaceous earth as a kind of water imbibition template, additive amount concentration is 1.0-200.0g/L, and dopamine is a kind of the organic of Nitrogen element
Monomer, additive amount concentration are 2.0-400.0g/L, and weakly alkaline solution concentration is 0.001-1.0mol/L, reaction time 6.0-
48.0 hours；The weakly alkaline solution refers to trishydroxymethylaminomethane aqueous solution.
3. a kind of preparation method of nitrogen oxygen codope porous carbon according to claim 1, which is characterized in that step B refers to
The material filter cake being obtained by filtration adds deionized water to filter elution at room temperature, or 55.0-85.0 DEG C of material filter cake baking being obtained by filtration
After dry plus deionized water filters elution at room temperature.
4. a kind of preparation method of nitrogen oxygen codope porous carbon according to claim 1, which is characterized in that alkali in step C
Property solution concentration be 1.0-12.0mol/L, soaking time be 0.05-48.0 hours；The alkaline solution is that potassium hydroxide is molten
Liquid.
5. a kind of preparation method of nitrogen oxygen codope porous carbon according to claim 1, which is characterized in that carbon in step D
Changing temperature is 400.0-1200.0 DEG C, and the time is 1.0-24.0 hours.
6. a kind of preparation method of nitrogen oxygen codope porous carbon according to claim 1, which is characterized in that alkali in step E
Property solution be sodium hydroxide or potassium hydroxide solution, concentration 5.0-15.0mol/L, reaction temperature be 100.0-300.0 DEG C, instead
It is 5.0-50.0 hours between seasonable.
7. a kind of preparation method of nitrogen oxygen codope porous carbon according to claim 1, which is characterized in that washed in step F
It washs and refers to that the material filter cake being obtained by filtration adds deionized water to filter elution at room temperature.
8. a kind of preparation method of nitrogen oxygen codope porous carbon according to claim 1, which is characterized in that done in step G
It is dry to refer to washed material filter cake through 55.0-85.0 DEG C of drying 5.0-10.0 hours or -50.0--90.0 DEG C of freezing vacuums of warp
It is 10-48.0 hours dry.
9. a kind of nitrogen oxygen codope porous carbon that method according to claim 1-8 is prepared.
10. a kind of application for nitrogen oxygen codope porous carbon that method according to claim 1-8 is prepared is made
For super capacitor material.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963877A (en) * | 2012-11-23 | 2013-03-13 | 中国科学院广州地球化学研究所 | Kieselguhr template carbon with large specific surface area and high pore volume and preparation method thereof |
| CN107572497A (en) * | 2017-09-26 | 2018-01-12 | 南京理工大学 | The preparation method of N doping grade hole carbon material |
| CN108773841A (en) * | 2018-06-26 | 2018-11-09 | 广西师范大学 | A kind of porous carbon materials and its preparation method and application prepared by discarded diatomite |
| CN109437156A (en) * | 2018-11-13 | 2019-03-08 | 上海师范大学 | A kind of preparation method of nitrogen-doped carbon nanometer pipe |
-
2019
- 2019-04-21 CN CN201910322860.XA patent/CN110085438A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963877A (en) * | 2012-11-23 | 2013-03-13 | 中国科学院广州地球化学研究所 | Kieselguhr template carbon with large specific surface area and high pore volume and preparation method thereof |
| CN107572497A (en) * | 2017-09-26 | 2018-01-12 | 南京理工大学 | The preparation method of N doping grade hole carbon material |
| CN108773841A (en) * | 2018-06-26 | 2018-11-09 | 广西师范大学 | A kind of porous carbon materials and its preparation method and application prepared by discarded diatomite |
| CN109437156A (en) * | 2018-11-13 | 2019-03-08 | 上海师范大学 | A kind of preparation method of nitrogen-doped carbon nanometer pipe |
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