CN109336094A - A kind of nitrogen-doped graphene and preparation method - Google Patents
A kind of nitrogen-doped graphene and preparation method Download PDFInfo
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- CN109336094A CN109336094A CN201811497909.7A CN201811497909A CN109336094A CN 109336094 A CN109336094 A CN 109336094A CN 201811497909 A CN201811497909 A CN 201811497909A CN 109336094 A CN109336094 A CN 109336094A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
Abstract
The invention discloses a kind of nitrogen-doped graphene and preparation method, include the following steps: to prepare graphene oxide；It is added in graphene oxide after deionized water and obtains graphene oxide dispersion by ultrasound and centrifugation, be put into reaction kettle after urea I ultrasound is added to graphene oxide dispersion, reaction temperature is 160 DEG C, reaction time 3h, and nitrogen-doped graphene I is made；It is put into autoclave after being mixed after melamine addition dehydrated alcohol with graphene oxide dispersion, reaction temperature is 180 DEG C, reaction time 8h, and nitrogen-doped graphene II is made；Graphene oxide dispersion, calcium chloride and the mixing of oxalic acid powder ultrasonic, thioacetamide is dissolved in deionized water ultrasonic mixing, the two is remixed ultrasonic vibration 1h is placed on electromagnetic oven and heat, and reaction temperature is 80 DEG C, reaction time is 6h, and nitrogen-doped graphene III is made.The nitrogen-doped graphene quality prepared by the preparation method that the invention provides is higher, and defect is reduced, and improves the comprehensive performance of N doping graphite.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials more particularly to a kind of nitrogen-doped graphene and preparation methods.
Background technique
Since graphene specific surface area is compared with high, intensity is big, thermal conductivity is high and the excellent properties such as good conductivity, in various fields
It is widely used, such as new energy, catalyst and biomedicine.Inertia is presented in the graphene surface of complete structure, generally
Method is by graphene and other elements or Material cladding, to obtain good comprehensive performance.
Chemical element doping is to improve one of the more efficient method of graphene performance.The side of nitrogen-doped graphene is prepared at present
Method mainly has: (1) chemical vapour deposition technique, which is to react gaseous precursor on matrix, forms film, and this method needs
Metallic catalyst is used, separating metallic catalyst and nitrogen-doped graphene are relatively difficult, and technique is more complex；(2) nitrogenous precursor
Transformation approach, the method are after mixing nitrogen substance with transition metal compound catalyst, to react at high temperature, remove metal compound
Nitrogen-doped graphene is obtained after object, metallic catalyst used in the method can generate metal carbides, it is difficult to thoroughly remove, influence
Later period uses；(3) graphene oxide nitriding, the method are using graphene oxide as raw material, using nitrogen substance as nitrogen source, in high temperature
Or nitrating under hydrothermal condition, the patent of Publication No. CN104465113 disclose the method that hydro-thermal method prepares nitrogen-doped graphene,
The method is after mixing with urea and sulfuric acid, in 180 DEG C of hydro-thermal reaction 2h, to obtain N doping graphite using graphene oxide as raw material
Alkene, since graphene oxide is not easy to obtain, higher cost, the method is restricted.
Since there are problems for the above method, as N doping amount is not high, graphene reduction rate is low, doped graphene defect
The features such as more.Therefore, seek that a kind of simple process, raw material is easy to get, cost is relatively low, without using the preparation side of metallic catalyst
Method has a very important significance.
Summary of the invention
The object of the invention is that providing a kind of preparation of high quality nitrogen-doped graphene to solve the above-mentioned problems
Method.
To achieve the goals above, the disclosure provides a kind of nitrogen-doped graphene and preparation method, includes the following steps:
S1: graphene oxide is prepared；
S2: it is added in graphene oxide after deionized water and obtains graphene oxide dispersion by ultrasound and centrifugation；
S3: urea is added to graphene oxide dispersion and obtains mixture I, is put into reaction kettle after mixture I ultrasound 30min
In, reaction temperature is 160 DEG C, reaction time 3h, and nitrogen-doped graphene I is made；
S4: melamine mixes to obtain mixtures II after dehydrated alcohol ultrasound 10min is added with graphene oxide dispersion, mixes
It is put into autoclave after closing object II ultrasound 30min, reaction temperature is 180 DEG C, reaction time 8h, and N doping graphite is made
Alkene II；
S5: mixtures III, thioacetamide are obtained after graphene oxide dispersion, calcium chloride and oxalic acid powder ultrasonic 30min
It is dissolved in deionized water ultrasound 30min and obtains mixture IV, mixtures III and mixture IV mixing ultrasonic vibration 1h are placed on electricity
It is heated on magnetic furnace, reaction temperature is 80 DEG C, reaction time 6h, and nitrogen-doped graphene III is made.
Optionally, S1 step specifically includes: measuring graphite powder, sodium nitrate and the concentrated sulfuric acid under condition of ice bath and is stirred to react
Afterwards, strong oxidizer is added, and is stirred at room temperature to discoloration, deionized water stirring is then added dropwise, stirs simultaneously thereto
Hydrogen peroxide reaction is added, is washed to solution with dilute hydrochloric acid and deionized water dry after being in neutrality after reaction, obtains graphene oxide.
Optionally, strong oxidizer is at least one of sulfuric acid, potassium permanganate, sodium nitrate.
Optionally, in S3, graphene oxide dispersion and urea are mixed with the ratio of 1mL:20mg.
Optionally, in S3, natural cooling after mixture I is heated in a kettle, then with dilute hydrochloric acid solution and going
Ion water washing to solution is in neutrality, and obtains that nitrogen-doped graphene I is made after dry.
Optionally, in S4, graphene oxide dispersion, dehydrated alcohol and melamine are mixed with the ratio of 1mL:1mL:4mg
It closes.
Optionally, in S4, mixtures II reacts natural cooling after 8h in a high pressure reaction kettle, then with dilute hydrochloric acid solution and
Deionized water is washed to solution and is in neutrality, and obtains nitrogen-doped graphene II after dry.
Optionally, in S5, graphene oxide dispersion, calcium chloride and oxalic acid powder are mixed with the ratio of 10mL:50mg:41mg
It closes to obtain mixtures III, thioacetamide and deionized water and mixture IV is mixed to obtain with the ratio of 50mg:5mL.
Optionally, in S5, mixtures III and the mixed mixed solution of mixture IV heat up on the electromagnetic oven of 1300W
When to 80 DEG C, 0.1molL is added dropwise dropwise-1Sodium hydroxide solution, so that the pH of mixed solution is adjusted to 10, continue to heat.
Optionally, in S5, after reacting 6h, the supernatant in container is outwelled, taking precipitate matter is washed with deionized more
After secondary, dried for 24 hours under conditions of 70 DEG C, and the compound after drying is dissolved in 5molL-1Hydrochloric acid solution in, stirring
And ultrasound 1h, then be washed with deionized to neutrality, drying for 24 hours, obtains nitrogen-doped graphene III at 60 DEG C after filtering.
The beneficial effects of the present invention are:
The present invention prepares graphene oxide by improveing Hummers method, produces nitrogen-doped graphene using hydro-thermal method, and phase
Prepared by nitrogen-doped graphene, such as chemical vapor deposition and arc discharge method for other methods, equipment needed for hydro-thermal method is simple,
Condition requirement is lower, is more suitable for preparing for laboratory.
Detailed description of the invention
Attached drawing is and to constitute part of specification for providing further understanding of the disclosure, with following tool
Body embodiment is used to explain the disclosure together, but does not constitute the limitation to the disclosure.In the accompanying drawings:
Fig. 1 is nitrogen-doped graphene I, nitrogen-doped graphene II, nitrogen-doped graphene III and graphene of the present invention
XRD diagram；
Fig. 2 is the Raman light of nitrogen-doped graphene I of the present invention, nitrogen-doped graphene II, nitrogen-doped graphene III
Spectrogram；
Fig. 3 is circulation volt of the nitrogen-doped graphene II of the present invention in potassium hydroxide solution under different scanning rates
Antu；
Fig. 4 is charging and discharging curve of the nitrogen-doped graphene II of the present invention under the current density of 1A/g.
Description of symbols
NG-1- nitrogen-doped graphene I, NG-2- nitrogen-doped graphene II, NG-3- nitrogen-doped graphene III, GR- graphite
Alkene.
Specific embodiment
It is described in detail below in conjunction with specific embodiment of the attached drawing to the disclosure.It should be understood that this place is retouched
The specific embodiment stated is only used for describing and explaining the disclosure, is not limited to the disclosure.
The present invention relates to a kind of nitrogen-doped graphenes and preparation method to include the following steps:
S1: graphene oxide is prepared；
S2: preparation graphene oxide dispersion；
S3: measuring graphene oxide dispersion, and nitrogen-doped graphene I is made by hydro-thermal method as nitrogen source in urea；
S4: measuring graphene oxide dispersion, and nitrogen-doped graphene II is made by hydro-thermal method as nitrogen source in melamine；
S5: measuring graphene oxide dispersion, and nitrogen-doped graphene is made by hydro-thermal method as nitrogen source in thioacetamide
III。
The particular content of S1 are as follows:
Firstly, 2.5g graphite powder and 1.25g sodium nitrate are added in 500mL beaker, secondly, the concentrated sulfuric acid of 58mL is added,
Mass fraction is 98%.Under conditions of 0 DEG C or so, obtained mixed solution is stirred into 2h；Secondly, under stirring conditions,
It is slowly added to 15g potassium permanganate into obtained mixture to be reacted, and keeps the temperature of reaction at 20 DEG C hereinafter, completing high
Ice bath device is removed after the addition of potassium manganate, obtained reaction product is stirred at room temperature, solution becomes bottle green from black
Paste；Then, 300mL deionized water is added dropwise into beaker under stiring, reaction temperature is rapidly increased to 95 DEG C, and generates
A large amount of bubbles, the color moment of solution becomes vivid yellow in beaker.Obtained product is stirred into 2h, Zhi Houjia at 95 DEG C
Enter the hydrogen peroxide that 50mL concentration is 30%, obtains the crude product of graphene oxide；Finally, by the thick production of obtained graphene oxide
Object with 5% dilute hydrochloric acid centrifuge washing three times, then be washed with deionized for several times, until stop washing when cleaning solution is neutral,
Obtained solid is dried, graphene oxide is obtained.
The particular content of S2 are as follows:
100mg graphene oxide solid is weighed, 100mL deionized water is added, after solution ultrasound 30min, then with
3500r/min is centrifuged 10min, and centrifugation is repeated as many times, and apparent bulky grain solid is removed, then take upper solution, with 5000r/min
It is centrifuged 10min, the solid for being centrifuged tube wall and bottom is distributed in water, the preferable dilute dispersion of 1mg/ml graphite oxide of quality is obtained
Liquid.
The particular content of S3 are as follows:
20mL graphene oxide dispersion is taken, 400mg urea, ultrasonic disperse 30min is added.Dispersion liquid is put into reaction kettle
In, heating temperature is to 160 DEG C, reaction time 3h, natural cooling after heating.First washed with the dilute hydrochloric acid that concentration is 5%
Coolant liquid is to remove alkali ion, then straight solution is washed with deionized repeatedly and is in neutrality, and after dry under conditions of 70 DEG C, obtains
To nitrogen-doped graphene I.
The particular content of S4 are as follows:
Measure 20mL graphene oxide dispersion, 20mL dehydrated alcohol, 80mg melamine.Nothing first is added in melamine
In water-ethanol, ultrasonic 10min, then mixed with graphene oxide dispersion, ultrasonic 30min.Mixed liquor is put into autoclave
In, reaction temperature is 180 DEG C, after reacting 8h, natural cooling.Gained black solid is washed three times with the dilute hydrochloric acid that concentration is 5%,
It is washed with deionized again later repeatedly to remove dilute hydrochloric acid, test solution stops washing when being neutral.By solid at 70 DEG C
Under the conditions of it is dry after, obtain nitrogen-doped graphene II.
The particular content of S5 are as follows:
100ml graphene oxide dispersion is taken, 0.5g calcium chloride and 0.41g oxalic acid powder, ultrasonic 30min is added.Meanwhile
0.5g thioacetamide is dissolved in 50mL deionized water, ultrasonic 30min.Two kinds of solution are uniformly mixed and ultrasound is shaken
Mixed solution, is put on the electromagnetic oven of 1300W heats later, when being warming up to 80 DEG C, 0.1molL is added dropwise dropwise by dynamic 1h-1's
Sodium hydroxide solution makes the pH of solution be adjusted to 10, continues to heat, and after reacting 6h, outwells supernatant, taking precipitate matter is used
Dry under conditions of 70 DEG C after deionized water washing repeatedly, the time is for 24 hours, to obtain nitrogen-doped graphene/oxalic acid calcium complexes.
Nitrogen-doped graphene obtained/oxalic acid calcium complexes are dissolved in 5molL-1Hydrochloric acid solution in, stir and ultrasound 1h, repeatedly wash
It washs three times, then is washed with deionized for several times to neutrality, filter, drying for 24 hours, obtains nitrogen-doped graphene III at subsequent 60 DEG C.
The present invention prepares graphene oxide by improveing Hummers method, and hydro-thermal method prepares nitrogen-doped graphene, is respectively adopted
Urea, melamine and thioacetamide are as nitrogen source redox graphene and carry out N doping, the system of nitrogen-doped graphene I
The standby time is most short, and nitrogen-doped graphene II is secondly, the two preparation process is relatively simple, and heating temperature is compared with nitrogen-doped graphene III
It is high.The preparation time longest of nitrogen-doped graphene III, preparation section is more, deposits and releases stink damp etc. during the preparation process and ask
Topic.
Graphene oxide obtained, nitrogen-doped graphene I, nitrogen-doped graphene II and nitrogen-doped graphene III are distinguished
Carry out X-ray diffraction analysis, Raman spectrum analysis, cyclic voltammetric analysis.
X-ray diffraction analysis:
As shown in Figure 1, nitrogen-doped graphene II relative to nitrogen-doped graphene I and nitrogen-doped graphene III interlamellar spacing most
Small and peak position is more obvious, so melamine makes graphene oxide restore more thorough, while graphite lattice structure is restored
Degree also highest.
Raman spectrum analysis:
As shown in Fig. 2, the ID/IG value of nitrogen-doped graphene II is minimum, and its peak is most narrow, shows that its defect is minimum, orderly
Spend higher, while the I2D/IG value of nitrogen-doped graphene II is maximum, shows that its number of plies in three is most thin, quality highest.
Cyclic voltammetric analysis:
As shown in figure 3, the cyclic voltammetric area of nitrogen-doped graphene II is maximum, and nitrogen is mixed under identical current density condition
The minimum of miscellaneous graphene I, nitrogen-doped graphene III be located between the two, therefore with nitrogen-doped graphene I and nitrogen-doped graphene
III is compared, and nitrogen-doped graphene II has bigger specific capacitance, and cycle life is best, and charging-discharging structure is stablized, to make super
Capacitor performance is more excellent.
Constant current charge-discharge analysis:
As shown in figure 4, the charging and discharging curve of nitrogen-doped graphene II shows relatively good under different current densities
Symmetry, therefore nitrogen-doped graphene II structure is more outstanding, charge-discharge performance is stablized, and possesses as modified electrode material good
Capacity retention has good electric double layer capacitance characteristic.
Analysis result Comprehensive Correlation shows under hydrothermal condition above, the oxidation using melamine as nitrogen source, with high quality
The nitrogen-doped graphene quality that graphene dispersing solution and ethanol synthesis 8h are obtained is best, and this method makes graphene oxide restore more
To be thorough, electric property is also the most excellent.
The preferred embodiment of the disclosure is described in detail in conjunction with attached drawing above, still, the disclosure is not limited to above-mentioned reality
The detail in mode is applied, in the range of the technology design of the disclosure, a variety of letters can be carried out to the technical solution of the disclosure
Monotropic type, these simple variants belong to the protection scope of the disclosure.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the disclosure to it is various can
No further explanation will be given for the combination of energy.
In addition, any combination can also be carried out between a variety of different embodiments of the disclosure, as long as it is without prejudice to originally
Disclosed thought equally should be considered as disclosure disclosure of that.
Claims (10)
1. a kind of nitrogen-doped graphene and preparation method, which is characterized in that include the following steps:
S1: graphene oxide is prepared；
S2: it is added in graphene oxide after deionized water and obtains graphene oxide dispersion by ultrasound and centrifugation；
S3: urea is added to graphene oxide dispersion and obtains mixture I, is put into reaction kettle after mixture I ultrasound 30min, instead
Answering temperature is 160 DEG C, reaction time 3h, and nitrogen-doped graphene I is made；
S4: melamine mixes to obtain mixtures II, mixture after dehydrated alcohol ultrasound 10min is added with graphene oxide dispersion
It is put into autoclave after II ultrasound 30min, reaction temperature is 180 DEG C, reaction time 8h, and nitrogen-doped graphene is made
II；
S5: mixtures III, thioacetamide dissolution are obtained after graphene oxide dispersion, calcium chloride and oxalic acid powder ultrasonic 30min
Mixture IV is obtained in deionized water ultrasound 30min, mixtures III and mixture IV mixing ultrasonic vibration 1h are placed on electromagnetic oven
Upper heating, reaction temperature are 80 DEG C, reaction time 6h, and nitrogen-doped graphene III is made.
2. a kind of nitrogen-doped graphene according to claim 1 and preparation method, which is characterized in that S1 step is specifically wrapped
It includes: after measurement graphite powder, sodium nitrate and the concentrated sulfuric acid are stirred to react under condition of ice bath, strong oxidizer is added, and stir at room temperature
It mixes to discoloration, deionized water stirring is then added dropwise, stirring is added hydrogen peroxide reaction thereto simultaneously, uses dilute hydrochloric acid after reaction
Drying after being in neutrality is washed to solution with deionized water, obtains graphene oxide.
3. a kind of nitrogen-doped graphene according to claim 2 and preparation method, it is characterised in that: strong oxidizer is sulphur
At least one of acid, potassium permanganate, sodium nitrate.
4. a kind of nitrogen-doped graphene according to claim 1 and preparation method, it is characterised in that: in S3, graphite oxide
Alkene dispersion liquid and urea are mixed with the ratio of 1mL:20mg.
5. a kind of nitrogen-doped graphene according to claim 1 and preparation method, it is characterised in that: in S3, mixture I exists
Natural cooling after heating in reaction kettle, is then washed to solution with dilute hydrochloric acid solution and deionized water and is in neutrality, after dry
It obtains that nitrogen-doped graphene I is made.
6. a kind of nitrogen-doped graphene according to claim 1 and preparation method, it is characterised in that: in S4, graphite oxide
Alkene dispersion liquid, dehydrated alcohol and melamine are mixed with the ratio of 1mL:1mL:4mg.
7. a kind of nitrogen-doped graphene according to claim 1 and preparation method, it is characterised in that: in S4, mixtures II
Natural cooling after reaction 8h in a high pressure reaction kettle, is then washed to solution with dilute hydrochloric acid solution and deionized water and is in neutrality, done
Nitrogen-doped graphene II is obtained after dry.
8. a kind of nitrogen-doped graphene and preparation method according to claim 1, it is characterised in that: in S5, graphene oxide
Dispersion liquid, calcium chloride and oxalic acid powder mix to obtain mixtures III with the ratio of 10mL:50mg:41mg, thioacetamide and go from
Sub- water mixes to obtain mixture IV with the ratio of 50mg:5mL.
9. a kind of nitrogen-doped graphene according to claim 1 and preparation method, it is characterised in that: in S5, mixtures III
With the mixed mixed solution of mixture IV when being warming up to 80 DEG C on the electromagnetic oven of 1300W, 0.1molL is added dropwise dropwise-1's
Sodium hydroxide solution makes the pH of mixed solution be adjusted to 10, continues to heat.
10. a kind of nitrogen-doped graphene according to claim 1 and preparation method, it is characterised in that: in S5, react 6h
Afterwards, the supernatant in container is outwelled, taking precipitate matter is dry under conditions of 70 DEG C after being washed with deionized repeatedly
For 24 hours, and by the compound after drying it is dissolved in 5molL-1Hydrochloric acid solution in, stir and ultrasound 1h, then be washed with deionized water
It washs to neutrality, drying for 24 hours, obtains nitrogen-doped graphene III at 60 DEG C after filtering.
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| CN112687902A (en) * | 2020-12-28 | 2021-04-20 | 龙岩学院 | Preparation method of nitrogen-doped graphene-supported hollow nano platinum composite material |
| CN114162808A (en) * | 2021-12-03 | 2022-03-11 | 北京蒙京石墨新材料科技研究院有限公司 | Nitrogen-doped graphene and preparation method and application thereof |
| CN114892451A (en) * | 2022-06-02 | 2022-08-12 | 山东东宇鸿翔装饰材料有限公司 | Copper-nitrogen doped TiO 2 Antibacterial paper, antibacterial board and preparation method thereof |
| CN115318268A (en) * | 2021-09-30 | 2022-11-11 | 湘潭大学 | Preparation method and application of nonmetallic catalyst for liquid-phase hydrogenation of nitroarene |
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