CN109626364A - A kind of preparation method of nitrogen sulphur codope three-dimensional grapheme - Google Patents
A kind of preparation method of nitrogen sulphur codope three-dimensional grapheme Download PDFInfo
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- CN109626364A CN109626364A CN201910084745.3A CN201910084745A CN109626364A CN 109626364 A CN109626364 A CN 109626364A CN 201910084745 A CN201910084745 A CN 201910084745A CN 109626364 A CN109626364 A CN 109626364A
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- C01B32/00—Carbon; Compounds thereof
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention discloses a kind of preparation methods of nitrogen sulphur codope three-dimensional grapheme, solve the problems such as prior art higher cost, complex process and yield are lower.The present invention, which mainly comprises the following steps, mixes carbon matrix precursor, solvent, dopant and template, carries out hydro-thermal reaction, is then carbonized, the techniques such as removing template is gone to prepare the porous graphene material with three-dimensional structure.Product specific surface area of the invention is 400~1500m2/ g, the number of plies are 3~20 layers, and resistivity is small (20~50 Ω m), and yield height (40~60%), pore-size distribution is more uniform；And manufacture craft is simple, and it is at low cost, it is easy to industrialized production.
Description
Technical field
The invention belongs to function nano Material Fields, and in particular to a kind of preparation side of nitrogen sulphur codope three-dimensional grapheme
Method.
Background technique
Graphene be one kind by carbon atom with sp2Hybridized orbit combines and the two-dimensional material of only monoatomic layer thickness, is
The basic unit for constituting carbonaceous material is answered extensively due to high conductivity, big specific surface area and its high heat conductivity
For in the devices such as fuel cell, supercapacitor, sensor, it has also become research hotspot.But conventional graphite alkene interlayer there is
Stronger Van der Waals force and π-pi bond, and cause graphene that irreversible stacking, fold and reunion, therefore electric conductivity and Bi Biao occurs
Area all decreases, therefore is unable to satisfy practical application request, limits its application to a certain extent.It is asked to solve this
Topic, building have a kind of nitrogen sulphur codope three-dimensional grapheme, (have using its unique porous structure and excellent internal performance
Biggish specific surface area, work long hours stability), to improve the electric property of graphene.
Currently, there are mainly two types of: 1. self-assembly methods for the preparation method of nitrogen sulphur codope three-dimensional grapheme, be it is a kind of from
The preparation method of nano material under above is added crosslinking agent, sends out in pyroreaction kettle generally using graphene oxide as raw material
Raw cross-linking reaction, to complete the self assembling process of three-dimensional grapheme.But the method be easy to cause environmental pollution, is unfavorable for producing greatly
Amount preparation, commercialization receive certain limitation.2. template, generally using copper, nickel, silver etc. as template, graphite is carbon source, system
It is standby go out three-dimensional netted graphene porosity with higher and big specific surface area, be conducive to diffusion and the ion of electrolyte
Transmission.But template used is the noble metals such as copper, nickel, silver, expensive, and the later period needs to perform etching template, from warp
The application of its large-scale commercial is limited in terms of Ji and environment.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of system of the nitrogen sulphur codope three-dimensional grapheme of low cost
Preparation Method, this method preparation process is simple, and raw material sources are abundant and cheap, obtains three-dimensional porous graphene, has
The advantages that large specific surface area, yield are high, and resistivity is small and good conductivity.
The specific technical proposal is:
A kind of preparation method of nitrogen sulphur codope three-dimensional grapheme, sequentially includes the following steps:
(1) carbon matrix precursor, solvent, dopant are added to reaction under high pressure according to 1~5:0.1 of mass ratio~10:0.1~5
It in kettle, stirs evenly, 4~8h is reacted at 120~200 DEG C；
(2) after being cooled to room temperature, template is added, template and carbon matrix precursor mass ratio are 0.1~5,60~120 DEG C of water
It is sufficiently washed after 2~4h of thermal response, takes out drying；
(3) raw material after drying is placed in atmosphere furnace, is then warming up to 800~1200 DEG C, predetermined temperature heat preservation 1~
3h；Wherein heating rate is 1~5 DEG C/min, and protective atmosphere is inert gas；
(4) product in step (3) is removed template: the product in step (3) is placed in acid and is stirred, through peracid
Wash, alcohol is washed and is washed to neutrality, is then put into 60~100 DEG C, be dried in vacuo 4~6h；It is wherein sour are as follows: hydrochloric acid, phosphoric acid, acetic acid,
One of sulfuric acid；The concentration of acid solution is 1~3mol/L.
Further, 5~50mg of carbon matrix precursor, 20~80mL of solvent, 2~20mg of dopant mixing in above-mentioned steps (1).
Further, carbon matrix precursor employed in above-mentioned steps (1) is sucrose, glucose, maltose, pitch, poly- second
One or more of alkene, polypropylene, polystyrene, phenolic resin, polyester resin, epoxy resin, glyceraldehyde.
Further, solvent employed in above-mentioned steps (1) be deionized water, ethyl alcohol, isopropanol, glycerol, n-butanol,
One of N, N- dimethyl pyrrolidone, ethylenediamine.
Further, dopant employed in above-mentioned steps (1) is thiocarbamide, methylthiouracil (MTU), propylthiouracil (PTU), first mercapto
One of imidazoles, Carbimazole, 4- plug oxazoline ketone, 2- substituted imine base -4- plug oxazoline ketone.
Further, template employed in above-mentioned steps (1) is magnesium chloride, magnesium sulfate, iron chloride, ferric nitrate, lemon
One of lemon acid iron, aluminium chloride, nano aluminium oxide, aluminium carbonate, nano silica.
Further, inert gas described in above-mentioned steps (3) is N2Or Ar2。
Beneficial effects of the present invention:
1. the specific surface area of nitrogen sulphur codope three-dimensional grapheme produced by the present invention is 400~1500m2/ g, the number of plies be 3~
20 layers, resistivity is small (20~50 Ω m), and yield height (40~60%), pore-size distribution is more uniform.
2. the present invention prepares nitrogen sulphur codope three-dimensional grapheme using cheap raw material, simple process is environmental-friendly,
Save the cost, it is easy to industrialized production.
3. using active metal oxide as template, and the later period is easy to pickling removal.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture of the nitrogen sulphur codope three-dimensional grapheme of 3 technique of embodiment preparation.
Fig. 2 is the scanning electron microscopic picture of the nitrogen sulphur codope three-dimensional grapheme of 5 technique of embodiment preparation.
Fig. 3 is that (note: embodiment 0 is for the resistivity map of the nitrogen sulphur codope three-dimensional grapheme of Examples 1 to 8 technique preparation
Three-dimensional grapheme undoped with nitrogen sulphur).
Fig. 4 is the yield figure of the nitrogen sulphur codope three-dimensional grapheme of Examples 1 to 8 technique preparation.
Specific embodiment
This paper way is further illustrated below in conjunction with specific embodiment, is embodied as follows:
Embodiment 1
20mg sucrose is added in the autoclave of 100mL, 5mg thiocarbamide is added as solvent in 45mL deionized water
It as nitrogen/sulphur source, is stirred, whipping temp is 80 DEG C, stirs 2h, and react 8h at 120 DEG C；It is to be cooled to after room temperature,
5mg nano aluminium oxide is then added, 70 DEG C of reaction 2h are washed with deionized repeatedly, and then 60 DEG C of vacuum drying 4h, are cooled to
Room temperature.Drying sample is put into atmosphere furnace, argon gas is passed through, 900 DEG C is warming up to 5 DEG C/min, keeps the temperature 3h, be cooled to room temperature and take
Out.Product is placed in hydrochloric acid solution (3mol/L), 1h is stirred, is washed till neutrality with deionized water and ethyl alcohol after being separated by filtration.
Dry 6h is placed in 70 DEG C of drying boxes.It can be obtained nitrogen sulphur codope three-dimensional grapheme, performance is as follows: specific surface area 750m2/
G, the number of plies are 3~10 layers；56 Ω m of resistivity, yield 40.3%；And SEM detection hole is more uniform.
Embodiment 2
10mg maltose is added in the autoclave of 100mL, 30mL glycerol is as solvent, 10mg methimazole,
It is stirred, whipping temp is 80 DEG C, stirs 2h, and react 6h at 130 DEG C；It is to be cooled to after room temperature, 6mg chlorine is then added
Change iron, 70 DEG C of reaction 2h are washed with deionized repeatedly, and then 60 DEG C of vacuum drying 4h, are cooled to room temperature.Drying sample is put
Enter in atmosphere furnace, be passed through argon gas, be warming up to 800 DEG C with 3 DEG C/min, keep the temperature 3h, is cooled to room temperature taking-up.Product is placed in salt
In acid solution (3mol/L), 1.5h is stirred, is washed till neutrality with deionized water and ethyl alcohol after being separated by filtration.It is placed in 70 DEG C of drying boxes
Middle dry 6h.It can be obtained nitrogen sulphur codope three-dimensional grapheme, performance is as follows: specific surface area 850m2/ g, the number of plies are 3~8 layers；
34.2 Ω m of resistivity, yield 38.4%；And SEM detection hole is more uniform.
Embodiment 3
15mg polyethylene is added in the autoclave of 100mL, 30mL glycerol is as solvent, 12mg methimazole,
It is stirred, whipping temp is 80 DEG C, stirs 1h, and react 6h at 150 DEG C；It is to be cooled to after room temperature, 5mg chlorine is then added
Change magnesium, 70 DEG C of reaction 2h are washed with deionized repeatedly, and then 60 DEG C of vacuum drying 6h, are cooled to room temperature.Drying sample is put
Enter in atmosphere furnace, be passed through argon gas, be warming up to 1000 DEG C with 2 DEG C/min, keep the temperature 2h, is cooled to room temperature taking-up.Product is placed in
In phosphoric acid solution (4mol/L), 1.5h is stirred, is washed till neutrality with deionized water and ethyl alcohol after being separated by filtration.It is placed in 80 DEG C of dryings
Dry 6h in case.It can be obtained nitrogen sulphur codope three-dimensional grapheme, performance is as follows: specific surface area 823m2/ g, the number of plies are 6~10
Layer；38.5 Ω m of resistivity, yield 45.2%；And SEM detection hole is more uniform.
Embodiment 4
15mg sucrose is added in the autoclave of 100mL, 30mL ethyl alcohol is as solvent, 10mg methylthiouracil (MTU),
It is stirred, whipping temp is 80 DEG C, stirs 2h, and react 6h at 150 DEG C；It is to be cooled to after room temperature, 5mg chlorine is then added
Change magnesium, 70 DEG C of reaction 2h are washed with deionized repeatedly, and then 60 DEG C of vacuum drying 6h, are cooled to room temperature.Drying sample is put
Enter in atmosphere furnace, be passed through argon gas, be warming up to 1200 DEG C with 2 DEG C/min, keep the temperature 2h, is cooled to room temperature taking-up.Carbonizing production is put
It is placed in phosphoric acid solution (5mol/L), stirs 1h, be washed till neutrality with deionized water and ethyl alcohol after being separated by filtration.80 DEG C are placed in do
Dry 6h in dry case.It can be obtained nitrogen sulphur codope three-dimensional grapheme, performance is as follows: specific surface area 895m2/ g, the number of plies be 5~
10 layers；26.5 Ω m of resistivity, yield 42.7%；And SEM detection hole is more uniform.
Embodiment 5
12mg glyceraldehyde is added in the autoclave of 100mL, 35mL ethyl alcohol is as solvent, 10mg methimazole,
It is stirred, whipping temp is 80 DEG C, stirs 1h, and react 6h at 150 DEG C；It is to be cooled to after room temperature, 10mg is then added
Ferric nitrate, 70 DEG C of reaction 2h are washed with deionized repeatedly, and then 70 DEG C of vacuum drying 6h, are cooled to room temperature.By drying sample
It is put into atmosphere furnace, is passed through argon gas, be warming up to 1200 DEG C with 1 DEG C/min, keep the temperature 2h, be cooled to room temperature taking-up.Product is placed
In nitric acid solution (3mol/L), 2h is stirred, is washed till neutrality with deionized water and ethyl alcohol after being separated by filtration.It is placed in 80 DEG C of dryings
Dry 4h in case.It can be obtained nitrogen sulphur codope three-dimensional grapheme, performance is as follows: specific surface area 855m2/ g, the number of plies are 6~10
Layer；35 Ω m of resistivity, yield 45.6%, yield 43%；And SEM detection hole is more uniform.
Embodiment 6
30mg phenolic resin is added in the autoclave of 100mL, 30mL deionized water is as solvent, the third mercapto of 10mg
Imidazoles is stirred, and whipping temp is 80 DEG C, stirs 1h, and react 6h at 120 DEG C；It is to be cooled to after room temperature, be then added
15mg magnesium chloride, 70 DEG C of reaction 2h are washed with deionized repeatedly, and then 60 DEG C of vacuum drying 6h, are cooled to room temperature.It will dry
Sample is put into atmosphere furnace, is passed through argon gas, is warming up to 1000 DEG C with 2 DEG C/min, is kept the temperature 3h, and room temperature taking-up is cooled to.By product
It is placed in hydrochloric acid acid solution (4mol/L), stirs 1 hour, be washed till neutrality with deionized water and ethyl alcohol after being separated by filtration.It places
The dry 6h in 80 DEG C of drying boxes.It can be obtained nitrogen sulphur codope three-dimensional grapheme, performance is as follows: specific surface area 903m2/ g, layer
Number is 3~6 layers；25.7 Ω m of resistivity, yield 50.3%；And SEM detection hole is more uniform.
Embodiment 7
20mg pitch is added in the autoclave of 100mL, 30mL Carbimazole is as solvent, 15mg thiocarbamide, into
Row stirring, whipping temp are 80 DEG C, stir 1h, and react 6h at 150 DEG C；It is to be cooled to receive to 10mg after room temperature, is then added
Rice aluminium oxide, 70 DEG C of reaction 2h are washed with deionized repeatedly, and then 70 DEG C of vacuum drying 6h, are cooled to room temperature.It will dry sample
Product are put into atmosphere furnace, are passed through argon gas, are warming up to 1200 DEG C with 1 DEG C/min, are kept the temperature 1h, and room temperature taking-up is cooled to.Product is put
It is placed in sulfuric acid solution (3mol/L), stirs 1h, be washed till neutrality with deionized water and ethyl alcohol after being separated by filtration.80 DEG C are placed in do
Dry 6h in dry case.It can be obtained nitrogen sulphur codope three-dimensional grapheme, performance is as follows: specific surface area 803m2/ g, the number of plies be 6~
10 layers；41.2 Ω m of resistivity, yield 44.5%；And SEM detection hole is more uniform.
Embodiment 8
25mg polyester resin is added in the autoclave of 100mL, 30mL glycerol is as solvent, 10mg first mercapto miaow
Azoles is stirred, and whipping temp is 80 DEG C, stirs 1h, and react 4h at 180 DEG C；It is to be cooled to after room temperature, be then added
10mg magnesium chloride, 70 DEG C of reaction 2h are washed with deionized repeatedly, and then 60 DEG C of vacuum drying 6h, are cooled to room temperature.It will dry
Sample is put into atmosphere furnace, is passed through argon gas, is warming up to 1000 DEG C with 2 DEG C/min, is kept the temperature 2h, and room temperature taking-up is cooled to.By product
It is placed in hydrochloric acid solution (4mol/L), stirs 1h, be washed till neutrality with deionized water and ethyl alcohol after being separated by filtration.It is placed in 80 DEG C
Dry 6h in drying box.It can be obtained nitrogen sulphur codope three-dimensional grapheme, performance is as follows: specific surface area 830m2/ g, the number of plies 5
~10 layers；35.5 Ω m of resistivity, yield 42.5%；And SEM detection hole is more uniform.
Claims (7)
1. a kind of preparation method of nitrogen sulphur codope three-dimensional grapheme, which is characterized in that comprise the following steps that
(1) carbon matrix precursor, solvent, dopant are added to autoclave according to 1~5:0.1 of mass ratio~10:0.1~5
In, it stirs evenly, 4~8h is reacted at 120~200 DEG C；
(2) after being cooled to room temperature, template is added, template and carbon matrix precursor mass ratio are that 0.1~5,60~120 DEG C of hydro-thermals are anti-
It is sufficiently washed after answering 2~4h, takes out drying；
(3) raw material after drying is placed in atmosphere furnace, is then warming up to 800~1200 DEG C, predetermined temperature keeps the temperature 1~3h；Its
Middle heating rate is 1~5 DEG C/min, and protective atmosphere is inert gas；
(4) product in step (3) is removed template: the product in step (3) being placed in acid and is stirred, through overpickling,
Neutrality is washed and be washed to alcohol, is then put into 60~100 DEG C, is dried in vacuo 4~6h；It is wherein sour are as follows: hydrochloric acid, phosphoric acid, acetic acid, sulfuric acid
One of；The concentration of acid solution is 1~3mol/L.
2. preparation method according to claim 1, it is characterised in that: 5~50mg of carbon matrix precursor, solvent 20 in step (1)
~80mL, 2~20mg of dopant mixing.
3. preparation method according to claim 1 or 2, it is characterised in that: carbon matrix precursor employed in step (1) is sugarcane
Sugar, glucose, maltose, pitch, polyethylene, polypropylene, polystyrene, phenolic resin, polyester resin, epoxy resin, glycerol
One or more of aldehyde.
4. preparation method according to claim 1 or 2, it is characterised in that: solvent employed in step (1) is deionization
Water, ethyl alcohol, isopropanol, glycerol, n-butanol, N, one of N- dimethyl pyrrolidone, ethylenediamine.
5. preparation method according to claim 1 or 2, it is characterised in that: dopant employed in step (1) is sulphur
Urea, methylthiouracil (MTU), propylthiouracil (PTU), methimazole, Carbimazole, 4- plug oxazoline ketone, 2- substituted imine base -4- fill in oxazoline ketone
One of.
6. preparation method according to claim 1 or 2, it is characterised in that: template employed in step (1) is chlorination
Magnesium, magnesium sulfate, iron chloride, ferric nitrate, ironic citrate, aluminium chloride, nano aluminium oxide, aluminium carbonate, one in nano silica
Kind.
7. preparation method according to claim 1 or 2, it is characterised in that: inert gas described in step (3) is N2Or
Ar2。
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| CN110010911A (en) * | 2019-03-14 | 2019-07-12 | 上海交通大学 | A kind of codope porous graphene cathode non-platinum catalyst and preparation method thereof |
| CN111940721A (en) * | 2020-08-19 | 2020-11-17 | 李潮云 | Method for loading nano metal oxide or nano metal material on porous carbon |
| CN112320797A (en) * | 2020-10-16 | 2021-02-05 | 中国科学院山西煤炭化学研究所 | Preparation method of activated carbon for desulfurization of tar hydrogenation product |
| CN112320792A (en) * | 2020-11-03 | 2021-02-05 | 青岛泰达华润新能源科技有限公司 | Preparation method of negative electrode material for lithium ion battery and product thereof |
| CN113735100A (en) * | 2021-09-07 | 2021-12-03 | 河北省科学院能源研究所 | Method for activating two-dimensional nitrogen-doped graphene |
| CN113877532A (en) * | 2021-11-15 | 2022-01-04 | 东北大学 | Graphene oxide reinforced solid waste inorganic spherical adsorbent, preparation method and application thereof |
| CN115010118A (en) * | 2022-06-06 | 2022-09-06 | 武汉理工大学 | Nitrogen and sulfur doped hierarchical macroporous/mesoporous graphene, and preparation method and application thereof |
| CN115849342A (en) * | 2022-12-26 | 2023-03-28 | 河北中煤旭阳能源有限公司 | Coiled nitrogen-sulfur-oxygen co-doped sodium ion battery negative electrode material and preparation method thereof |
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| CN110010911A (en) * | 2019-03-14 | 2019-07-12 | 上海交通大学 | A kind of codope porous graphene cathode non-platinum catalyst and preparation method thereof |
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| CN112320792A (en) * | 2020-11-03 | 2021-02-05 | 青岛泰达华润新能源科技有限公司 | Preparation method of negative electrode material for lithium ion battery and product thereof |
| CN112320792B (en) * | 2020-11-03 | 2023-03-24 | 青岛泰达华润新能源科技有限公司 | Preparation method of negative electrode material for lithium ion battery and product thereof |
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| CN113877532A (en) * | 2021-11-15 | 2022-01-04 | 东北大学 | Graphene oxide reinforced solid waste inorganic spherical adsorbent, preparation method and application thereof |
| CN113877532B (en) * | 2021-11-15 | 2023-07-18 | 东北大学 | Graphene oxide reinforced solid waste inorganic spherical adsorbent, preparation method and application thereof |
| CN115010118A (en) * | 2022-06-06 | 2022-09-06 | 武汉理工大学 | Nitrogen and sulfur doped hierarchical macroporous/mesoporous graphene, and preparation method and application thereof |
| CN115010118B (en) * | 2022-06-06 | 2024-01-23 | 武汉理工大学 | Nitrogen and sulfur doped hierarchical macroporous/mesoporous graphene and preparation method and application thereof |
| CN115849342A (en) * | 2022-12-26 | 2023-03-28 | 河北中煤旭阳能源有限公司 | Coiled nitrogen-sulfur-oxygen co-doped sodium ion battery negative electrode material and preparation method thereof |
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