CN107500267A - A kind of preparation method of the hollow carbosphere of N doping - Google Patents
A kind of preparation method of the hollow carbosphere of N doping Download PDFInfo
- Publication number
- CN107500267A CN107500267A CN201710967783.4A CN201710967783A CN107500267A CN 107500267 A CN107500267 A CN 107500267A CN 201710967783 A CN201710967783 A CN 201710967783A CN 107500267 A CN107500267 A CN 107500267A
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- China
- Prior art keywords
- doping
- preparation
- hollow
- carbosphere
- hollow carbosphere
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Cosmetics (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
A kind of preparation method of the hollow carbosphere of N doping.The present invention, through calcium chloride, after potassium carbonate pretreatment, is carbonized using starch as raw material in nitrogen, and is passed through ammonia in carbonisation and carries out N doping, and the carbon material of synthesis has hollow structure, and this method is simply easy to large-scale production.
Description
Technical field
The invention belongs to Material Field, and in particular to the preparation method of the hollow carbosphere of N doping a kind of.
Background technology
Carbon material has different morphologies, including one-dimensional CNT, the graphene of two dimension, network-like three-dimensional structure, ball
Shape carbon material and hollow spherical carbon material.Hollow spherical carbon material is due to its unique architectural feature, as electrode
The transmission range of electrolyte can significantly be shortened during material, so as to improve the chemical property of material.And after adulterating nitrogen in carbon ball
The chemical property of material can further be lifted.
The preparation method of hollow carbon balls is mainly solidifying including activation method, template, hydro-thermal method, chemical vapour deposition technique, carbonization
Glue method etc., most commonly template, the present invention develop a kind of no template in-situ activation and form porous hollow carbosphere.
The content of the invention
Present invention N doping hollow carbosphere with template-free method one-step synthesis.
Technical scheme is as follows：
Weigh 6 grams of starch to be placed in the certain density calcium chloride solutions of 100mL, soaking at room temperature 24 hours, filtering gained is filtered
Cake immerses in the solution of potassium carbonate again, adjusts pH value, filtration drying after soaking 24 hours, dried sample is put into tube furnace
800 DEG C are warming up under middle nitrogen atmosphere, constant temperature is passed through ammonia after 2 hours, cooling, with distillation water washing after 2mol/L chlorohydric acid picklings
To neutrality, the hollow carbosphere of N doping is obtained after filtration drying.
The concentration range of heretofore described calcium chloride solution is：0.1~1.5mol/L.
The concentration of heretofore described potassium carbonate is：0.01~1.0mol/L.
Heretofore described pH value is 9~12.
It is heretofore described be passed through ammonia time be：0~30 minute.
The preparation method of the hollow carbosphere of heretofore described N doping is simply easy to large-scale production.
Brief description of the drawings
Fig. 1 is the scanning electron microscopic picture of the hollow carbosphere of N doping prepared in embodiment 1；
Fig. 2 is the scanning electron microscopic picture of the hollow carbosphere of N doping prepared in embodiment 2.
Embodiment
Embodiment 1
Weigh 6 grams of starch to be placed in 100mL0.5mol/L calcium chloride solution, soaking at room temperature 24 hours, filtering gained is filtered
Cake immerses in the solution of 0.5mol/L potassium carbonate again, and regulation pH value is 9, filtration drying after soaking 24 hours, dried sample
Product, which are put into tube furnace, is warming up to 800 DEG C under nitrogen atmosphere, constant temperature is passed through ammonia 10 minutes after 2 hours, cooling, 2mol/L hydrochloric acid
Neutrality is washed with distilled water to after pickling, the hollow carbosphere of N doping is obtained after filtration drying.Accompanying drawing 1 shows prepared carbon materials
Material is in hollow sphere, and XPS test results show that the mass percent of nitrogen is 2.1%.
Embodiment 2
Weigh 6 grams of starch to be placed in 100mL1.0mol/L calcium chloride solution, soaking at room temperature 24 hours, filtering gained is filtered
Cake immerses in the cushioning liquid of 0.10mol/L potassium carbonate again, and regulation pH value is 11, filtration drying after soaking 24 hours, dry
Sample afterwards, which is put into tube furnace, is warming up to 800 DEG C under nitrogen atmosphere, constant temperature is passed through ammonia 20 minutes after 2 hours, cooling,
Neutrality is washed with distilled water to after 2mol/L chlorohydric acid picklings, the hollow carbosphere of N doping is obtained after filtration drying.Accompanying drawing 2 shows institute
The carbon material of preparation is in hollow sphere, and XPS test results show that the mass percent of nitrogen is 3.2%.
Claims (5)
1. a kind of preparation method of N doping hollow carbon pipe, it is characterised in that weighing 6 gram quantity starch mosses, to be placed in 100mL certain
In the calcium chloride solution of concentration, soaking at room temperature 24 hours, filtering gained filter cake immerses in the cushioning liquid of potassium carbonate again, adjusts pH
Value, filtration drying after soaking 24 hours, dried sample is put into tube furnace and 800 DEG C is warming up under nitrogen atmosphere, constant temperature 2
Ammonia is passed through after hour, is cooled down, neutrality is washed with distilled water to after 2mol/L chlorohydric acid picklings, is obtained after filtration drying in N doping
Empty carbosphere.
A kind of 2. preparation method of the hollow carbosphere of N doping according to claims 1, it is characterised in that the calcium chloride
The concentration range of solution is：0.1~1.5mol/L.
A kind of 3. preparation method of the hollow carbosphere of N doping according to claims 1, it is characterised in that the potassium carbonate
Concentration be：0.01~1.0mol/L.
4. a kind of preparation method of the hollow carbosphere of N doping according to claims 1, it is characterised in that the pH value is 9
~12.
5. a kind of preparation method of the hollow carbosphere of N doping according to claims 1, it is characterised in that described to be passed through ammonia
The time of gas is：0~30 minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710967783.4A CN107500267A (en) | 2017-10-17 | 2017-10-17 | A kind of preparation method of the hollow carbosphere of N doping |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710967783.4A CN107500267A (en) | 2017-10-17 | 2017-10-17 | A kind of preparation method of the hollow carbosphere of N doping |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107500267A true CN107500267A (en) | 2017-12-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710967783.4A Pending CN107500267A (en) | 2017-10-17 | 2017-10-17 | A kind of preparation method of the hollow carbosphere of N doping |
Country Status (1)
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| CN (1) | CN107500267A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325551A (en) * | 2018-01-29 | 2018-07-27 | 山东科技大学 | A kind of carbon-based transition-metal catalyst of N doping and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106379881A (en) * | 2016-09-12 | 2017-02-08 | 天津工业大学 | Preparation method of nitrogen-doped porous carbon spheres for neutral electrolyte supercapacitor |
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2017
- 2017-10-17 CN CN201710967783.4A patent/CN107500267A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106379881A (en) * | 2016-09-12 | 2017-02-08 | 天津工业大学 | Preparation method of nitrogen-doped porous carbon spheres for neutral electrolyte supercapacitor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325551A (en) * | 2018-01-29 | 2018-07-27 | 山东科技大学 | A kind of carbon-based transition-metal catalyst of N doping and preparation method thereof |
| CN108325551B (en) * | 2018-01-29 | 2020-09-01 | 山东科技大学 | Nitrogen-doped carbon-based transition metal catalyst and preparation method thereof |
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| PB01 | Publication | ||
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Application publication date: 20171222 |