CN108717979A - A kind of preparation method of the micro-nano carbon ball of N doping - Google Patents
A kind of preparation method of the micro-nano carbon ball of N doping Download PDFInfo
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- CN108717979A CN108717979A CN201810377431.8A CN201810377431A CN108717979A CN 108717979 A CN108717979 A CN 108717979A CN 201810377431 A CN201810377431 A CN 201810377431A CN 108717979 A CN108717979 A CN 108717979A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9091—Unsupported catalytic particles; loose particulate catalytic materials, e.g. in fluidised state
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a kind of preparation methods of the micro-nano carbon ball of N doping, and in particular to for one kind using glucose solution as carbon source, melamine is after nitrogen source mixes, at an appropriate reaction temperature, to synthesize the other N doping carbon ball of micro/nano level using hydro-thermal reaction technology.Raw material of the present invention is cheap, is easy to get, green.It is easily-controllable to test synthesis condition simplicity.The synthetic technology synthesizes the micro-nano carbon ball of the different N doping of size by conditions such as the concentration, the dosage of melamine and reaction temperature, reaction time of control glucose.The micro Nano material can be used for the application fields such as redox reactions in fuel cell (ORR), catalyst carrier, electrochemical device structure.
Description
Technical field
The present invention relates to a kind of preparation methods of novel micro-nano N doping carbon ball, and in particular to is with glucose solution
Carbon source, melamine are after nitrogen source mixes, at an appropriate reaction temperature, to synthesize micro-nano rank using hydro-thermal reaction technology
N doping carbon ball, belong to materials synthesis chemical field.
Background technology
In order to solve the problems, such as that electrode catalyst is unstable during fuel cells applications, Novel Carbon Nanomaterials such as carbon is received
Mitron, graphene etc. are received significant attention as the carrier material of carried noble metal.In the recent period, research finds nitrogen-doped carbon nanometer material
Material shows redox reactions (ORR) excellent electro-catalysis reduction activation, extremely strong to the anti-interference ability of methanol and have
Preferable stability.Nitrogen-doped carbon nano material has good electronic conduction ability, strong corrosion resistance, environmental-friendly and high
The characteristics such as specific surface area, in catalyst carrier, absorption, gas sensor, the processing of waste water organic dyestuff, electrochemical device structure
Aspect has potential application prospect.The method of synthesis nitrogen-doped carbon sill includes that chemical vapour deposition technique, high temperature move back at present
The synthetic technologys such as pyrogenic process, plasma method, hydro-thermal method, each have their own advantage and disadvantage of these preparation methods, generally existing experiment condition phase
The shortcomings of harshness and expensive instrument and reagent, material morphology and size are difficult to control, therefore a kind of green, simplicity of searching,
Controllable synthetic reaction technology, preparing the nitrogen-doped carbon sill that uniform pattern, structure and performance are stablized becomes current research
Hot spot.
Invention content
In order to solve above-mentioned deficiency in the prior art, the present invention provides one kind for the first time using glucose as carbon source, inexpensively
Melamine be nitrogen source, the controllable N doping of pattern, size is successfully synthesized using easily operated hydrothermal synthesis technology
The preparation method of micro-nano carbon ball.Primary Study reaction temperature, Concentration of precursor solution, reaction time are to synthetic material pattern, ruler
Very little influence, it is proposed that best synthetic technological condition.
To achieve the goals above, present invention employs technical solutions below：
A kind of preparation method of the micro-nano carbon ball of N doping, the melamine larger using cheap nitrogenous abundance is as nitrogen
The glucose solution in source, debita spissitudo is reaction solution, at a proper temperature, using easy easily operated hydro-thermal reaction method
Synthesize the relatively uniform N doping micro-nano carbon ball material of size.
The synthetic method is using melamine and glucose mixed solution as precursor liquid.
The synthetic method is synthesis vessel with pyroreaction kettle, using hydrothermal reaction condition, reaction temperature：160-
200 DEG C, the reaction time controls in 6-10h.
The glucose concentration：0.5-1mol/L, a concentration of 0.003-0.004g/mL of melamine solution.
Positive beneficial effect：Reaction raw materials used in the present invention all laboratories are common, it is cheap, be easy to get, nontoxic reagent.
An air dry oven is only needed in technical solutions according to the invention, the pyroreaction kettle of certain amount is experiment condition, is adopted
With the hydro-thermal reaction technology of relative low temperature, preparation method is simple and easy to do, and operating process is easily controllable, and the technology of preparing is easy to spread
It uses.
Description of the drawings：
The micro-nano carbon ball scanning electron microscope (SEM) photograph of Fig. 1 N dopings；
The micro-nano carbon ball EDS energy spectrum analysis figures of Fig. 2 N dopings.
Specific implementation mode
Embodiment 1
2.71g or so glucose is pipetted respectively to be dissolved in the deionized water of 15mL, then weighs the three of 0.005g or so
Poly cyanamid is dissolved in above-mentioned glucose solution, is uniformly mixed.Mixed solution is transferred to the high temperature hydro-thermal reaction of 25mL
In kettle, then reaction kettle is placed in drying box, setting reaction temperature is 180 DEG C, reaction time 3h.It waits for after reaction,
It is cooled to room temperature taking-up reaction kettle, after reaction solution centrifugal sedimentation is washed, sepia solid material is obtained, places it in 80 DEG C of bakings
It is dried in case, you can prepare N doping micro-nano carbon ball material.
Embodiment 2
2.71g or so glucose is pipetted respectively to be dissolved in the deionized water of 15mL, then weighs the three of 0.005g or so
Poly cyanamid is dissolved in above-mentioned glucose solution, is uniformly mixed.Mixed solution is transferred to the high temperature hydro-thermal reaction of 25mL
In kettle, then reaction kettle is placed in drying box, setting reaction temperature is 180 DEG C, reaction time 6h.It waits for after reaction,
It is cooled to room temperature taking-up reaction kettle, after reaction solution centrifugal sedimentation is washed, sepia solid material is obtained, places it in 80 DEG C of bakings
It is dried in case, you can prepare N doping micro-nano carbon ball material.
Embodiment 3
1.35g or so glucose is pipetted respectively to be dissolved in the deionized water of 15mL, then weighs the three of 0.005g or so
Poly cyanamid is dissolved in above-mentioned glucose solution, is uniformly mixed.Mixed solution is transferred to the high temperature hydro-thermal reaction of 25mL
In kettle, then reaction kettle is placed in drying box, setting reaction temperature is 180 DEG C, reaction time 3h.It waits for after reaction,
It is cooled to room temperature taking-up reaction kettle, after reaction solution centrifugal sedimentation is washed, sepia solid material is obtained, places it in 80 DEG C of bakings
It is dried in case, you can prepare N doping micro-nano carbon ball material.
The method of the invention prepares N doping micro-nano carbon ball material, is not limited to the above embodiment.According to the present invention
The characterization of the micro-nano carbon ball of N doping of the method synthesis is shown in shown in attached drawing 1-2
Reaction raw materials used in the present invention all laboratories are common, it is cheap, be easy to get, nontoxic reagent.It is of the present invention
An air dry oven is only needed in technical solution, the pyroreaction kettle of certain amount is experiment condition, using relative low temperature
Hydro-thermal reaction technology, preparation method is simple and easy to do, and operating process is easily controllable, technology of preparing use easy to spread.
Claims (3)
1. a kind of preparation method of the micro-nano carbon ball of N doping, it is characterised in that：It is higher with cheap glucose and nitrogen abundance
Melamine is raw material, can synthesize size difference at an appropriate reaction temperature using easy easily-controllable hydrothermal reaction condition
The micro-nano carbon ball of N doping.
2. a kind of preparation method of the micro-nano carbon ball of N doping according to claim 1, it is characterised in that：The nitrogen is mixed
Miscellaneous raw material is the cheap and higher melamine of nitrogen abundance.
3. a kind of preparation method of the micro-nano carbon ball of N doping according to claim 1, it is characterised in that：The reaction
Condition is：Hydrothermal reaction condition, the reaction time, reaction temperature was 150-200 DEG C in 3-6h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810377431.8A CN108717979A (en) | 2018-04-25 | 2018-04-25 | A kind of preparation method of the micro-nano carbon ball of N doping |
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| CN201810377431.8A CN108717979A (en) | 2018-04-25 | 2018-04-25 | A kind of preparation method of the micro-nano carbon ball of N doping |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110048107A (en) * | 2019-04-24 | 2019-07-23 | 陕西科技大学 | A kind of preparation method of self-supporting N doping hard carbon cathode material |
| CN111514852A (en) * | 2020-04-29 | 2020-08-11 | 广州大学 | Method for preparing nitrogen-doped carbon adsorbent by gas-phase hydrothermal carbonization of eutectic solvent |
| CN112206800A (en) * | 2020-08-31 | 2021-01-12 | 浙江工业大学 | Nitrogen-sulfur doped carbon material supported palladium catalyst, preparation method thereof and application thereof in tetrahydrophthalic anhydride hydrogenation reaction |
| CN112717725A (en) * | 2020-12-21 | 2021-04-30 | 太原理工大学 | Preparation method and application of mixed matrix carbon molecular sieve membrane doped with porous nitrogen-containing microspheres |
| CN113644269A (en) * | 2021-08-09 | 2021-11-12 | 西南大学 | Preparation method of nitrogen-doped hard carbon material, product and application thereof |
| CN114392765A (en) * | 2021-12-27 | 2022-04-26 | 河南师范大学 | Nitrogen-doped PHCS-Zn2In2S5Composite photocatalyst, preparation method and application thereof |
| CN115285968A (en) * | 2022-07-29 | 2022-11-04 | 东北林业大学 | Method for preparing cellulose carbon nanospheres by adopting o-phenylenediamine and application |
-
2018
- 2018-04-25 CN CN201810377431.8A patent/CN108717979A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110048107A (en) * | 2019-04-24 | 2019-07-23 | 陕西科技大学 | A kind of preparation method of self-supporting N doping hard carbon cathode material |
| CN111514852A (en) * | 2020-04-29 | 2020-08-11 | 广州大学 | Method for preparing nitrogen-doped carbon adsorbent by gas-phase hydrothermal carbonization of eutectic solvent |
| CN111514852B (en) * | 2020-04-29 | 2022-04-19 | 广州大学 | Method for preparing nitrogen-doped carbon adsorbent by gas-phase hydrothermal carbonization of eutectic solvent |
| CN112206800A (en) * | 2020-08-31 | 2021-01-12 | 浙江工业大学 | Nitrogen-sulfur doped carbon material supported palladium catalyst, preparation method thereof and application thereof in tetrahydrophthalic anhydride hydrogenation reaction |
| CN112717725A (en) * | 2020-12-21 | 2021-04-30 | 太原理工大学 | Preparation method and application of mixed matrix carbon molecular sieve membrane doped with porous nitrogen-containing microspheres |
| CN112717725B (en) * | 2020-12-21 | 2022-04-12 | 太原理工大学 | Preparation method and application of mixed matrix carbon molecular sieve membrane doped with porous nitrogen-containing microspheres |
| CN113644269A (en) * | 2021-08-09 | 2021-11-12 | 西南大学 | Preparation method of nitrogen-doped hard carbon material, product and application thereof |
| CN114392765A (en) * | 2021-12-27 | 2022-04-26 | 河南师范大学 | Nitrogen-doped PHCS-Zn2In2S5Composite photocatalyst, preparation method and application thereof |
| CN114392765B (en) * | 2021-12-27 | 2024-02-02 | 河南师范大学 | Nitrogen doped PHCS-Zn 2 In 2 S 5 Composite photocatalyst, preparation method and application thereof |
| CN115285968A (en) * | 2022-07-29 | 2022-11-04 | 东北林业大学 | Method for preparing cellulose carbon nanospheres by adopting o-phenylenediamine and application |
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Application publication date: 20181030 |