CN109573976A - A kind of nitrating porous carbon and its preparation method and application - Google Patents
A kind of nitrating porous carbon and its preparation method and application Download PDFInfo
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- CN109573976A CN109573976A CN201811325564.7A CN201811325564A CN109573976A CN 109573976 A CN109573976 A CN 109573976A CN 201811325564 A CN201811325564 A CN 201811325564A CN 109573976 A CN109573976 A CN 109573976A
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Abstract
The present invention relates to technical field of nano material more particularly to a kind of nitrating porous carbon and its preparation method and application.The method for preparing nitrating porous carbon is the following steps are included: S1: mung bean flour being added to the water, after mixing evenly, activator is added and urea obtains mixed liquor；S2: the mixed liquor that S1 is obtained is stirred, and sufficiently after reaction, re-dry obtains reactant；S3: reactant obtained in S2 is calcined under atmosphere of inert gases, sour processing is carried out after calcining again, obtains nitrating porous carbon.The raw material of this method are easy to get, are nontoxic, is at low cost；Next is not required to template, and activator calcium chloride is non-corrosive；Furthermore preparation flow is simple, equipment requirement is low, process is environmentally friendly, is suitble to large-scale promote and apply.Nitrating porous carbon is prepared with biggish specific surface area and a large amount of pore structure, function admirable by simple pyrolysismethod using mung bean flour as raw material.
Description
Technical field
The present invention relates to technical field of nano material more particularly to a kind of nitrating porous carbon and its preparation method and application.
Background technique
Carbon-based material in hardness, optical characteristics, heat resistance, radiation hardness characteristic, chemical-resistant resistance characteristic, electrical insulating property, lead
Electrically, surface and interfacial characteristics etc. have excellent performance, in related fieldss such as mechanics, the energy, electronic device, catalysis
Widely paid close attention to.
Wherein, porous material refers to the carbon material with certain pore structure, according to point of chemical combined meeting (IUPAC)
Porous material is divided into three classes by class: large pore material of the aperture less than the poromerics of 2nm, aperture greater than 50nm and between 2~
The mesoporous material of 50nm.Porous material have high-specific surface area, high heat conductance, high conductivity, high stability, high chemical inertness and
The advantages that low-density, before having wide application in fields such as supercapacitor, catalytic carrier, organic biomolecules absorption carriers
Scape.
The study found that if suitably adulterating other elements in carbon material, thus it is possible to vary the crystal structure and electricity of carbon material
Minor structure, to make its physics, chemical property better than common carbon material.Heteroatom doping can promote carbon material performance, expand
Its application potential in energy storage, conversion equipment.Nitrating meso-porous carbon material shows significantly to be catalyzed oxygen also in lye
Former reactivity and high supercapacitor specific capacitance [Liang Qunying, Su Hong, Yan Jing wait to be catalyzed journal, 2014,35 (7):
1078-1083.]。
Although the carbon material of N doping, since its excellent performance is increasingly interested by researchers, traditional nitrogen is mixed
Miscellaneous material is generally using expensive organic compound as raw material, based on complicated organic synthesis, under severe reaction conditions
It is prepared by high temperature cabonization, although can also obtain preferable effect, step is complex, therefore is difficult to be commercially produced
[Zhou Tianbao Northwest Normal University, 2014.].
With going deep into for Green Chemistry and sustainable development idea, how to be closed with cheap raw material by simple green method
The hot spot of research is had become at novel nitrogen-doped carbon material.Biomass presoma is from a wealth of sources, environmental-friendly, reserves and production
It measures huge, biomass efficient is converted into biomass-based carbon material, there is wide exploitation prospect.
The activation method of biomass carbon material is broadly divided into three kinds, is physical activation method, chemical activation method and physico respectively
Learn co-activating.Physical activation method is heated using vapor or carbon dioxide atmosphere, and advantage is mild condition, equipment requirement
Low, no coupling product after activation, no pollution to the environment, disadvantage is activation temperature height, and the time is long, and energy consumption is high；Chemical activation method leads to
The mode for crossing dipping infiltration activates carbon material, and advantage is that activation temperature is low, the time is short, the carbon materials of low energy consumption, preparation
Expect that specific surface area and hole appearance are larger, disadvantage, which is to have in big activator level, corrosion equipment, pollution environment and material, not to be removed
Activator.Physical chemistry co-activating includes a step chemical activation (usually using H3PO4And ZnCl2) and one-step physical activation it is (logical
It is often used CO2) process, but some inherent defects of do not have clear improvement physical activation method and chemical activation method.
Therefore, it is badly in need of developing that a kind of activation temperature is low, the time is short, low energy consumption, environmental-friendly, corrosivity is low and operates letter
Just the technology of preparing of biomass nitrating porous carbon.
Summary of the invention
In view of the above problems, the invention discloses a kind of nitrating porous carbon, specific scheme is as follows:
A kind of preparation method of nitrating porous carbon, comprising the following steps:
S1: mung bean flour is added to the water, and after mixing evenly, adds activator and urea obtains mixed liquor；
S2: the mixed liquor that S1 is obtained is stirred, and sufficiently after reaction, re-dry obtains reactant；
S3: reactant obtained in S2 is calcined under atmosphere of inert gases, sour processing is carried out after calcining again, obtains
Nitrating porous carbon.
It further, also successively include suction filtration, washing and drying steps after the completion of acid processing in S3.
Further, in S1, the activator is calcium chloride.
Further, in S1, stirring condition setting are as follows: whipping temp is 80 DEG C, and mixing time is 0.5~3h.
Further, in S1, mixing time 1h.
Further, in S1, the mass ratio of the mung bean flour and the activator is 1:(1~4).
Further, in S1, the mass ratio of the mung bean flour and the activator is 1:2.
Further, in S1, the mass ratio of the mung bean flour and the urea is 1:(1~3).
Further, in S1, the mass ratio of the mung bean flour and the urea is 1:2.
Calcine technology parameter includes calcination temperature, heating rate and calcination time etc., these parameters can all directly affect most
Throughout one's life at nitrating porous carbon quality.In the present invention, further, in S3, the program of the calcining is arranged are as follows: with 5 DEG C/
The heating rate of min is warming up to 700~900 DEG C, soaking time 2h.Calcination parameter is comprehensively considered to the shadow of nitrating porous carbon
It rings, it is preferred that temperature program when calcining are as follows: be warming up to 800 DEG C with the heating rate of 5 DEG C/min, calcination time 2h.
Further, in S3, the sour treatment process are as follows: use inorganic acid pickling at normal temperature；The inorganic acid is
One of hydrochloric acid, nitric acid, sulfuric acid or any combination thereof；The concentration of the inorganic acid is 0.5-2mol/L.The mesh of acid processing
Be remove the metal oxide that generates in calcination process, to form nitrating porous carbon.
The second aspect of the present invention provides the nitrating porous carbon that the above method is prepared.
Third aspect of the present invention provides application of the above-mentioned nitrating porous carbon in electrochemical field.
Compared with prior art, the invention has the following advantages:
(1) the nitrating porous carbon using mung bean flour as raw material is prepared by simple pyrolysismethod in the present invention, and traditional
Preparation method is compared, and the raw material of this method are easy to get, are nontoxic, is at low cost, next is not required to template, and activator chlorine
Change calcium is non-corrosive, and furthermore preparation flow is simple, equipment requirement is low, process is environmentally friendly, is suitble to large-scale promote and apply.
(2) preparation method of the present invention obtain using mung bean flour as the nitrating porous carbon of raw material have biggish specific surface area and
A large amount of pore structure.And the doping of nitrogen can greatly improve the performance of porous carbon materials, in electrochemistry, catalysis, energy field
In have broad application prospects.
Detailed description of the invention
The present invention will be further described with reference to the accompanying drawings, but the embodiment in attached drawing is not constituted to any limit of the invention
System.
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of nitrating porous carbon obtained in embodiment 1；
Fig. 2 is the nitrogen adsorption desorption curve of nitrating porous carbon obtained in embodiment 1；
Fig. 3 is the cyclic voltammogram of nitrating porous carbon obtained in Examples 1 to 3；
Fig. 4 is the scanning electron microscope (SEM) photograph (SEM) of nitrating porous carbon obtained in embodiment 2；
Fig. 5 is the nitrogen adsorption desorption curve of nitrating porous carbon obtained in embodiment 2.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments be only used for the present invention without
For limiting the scope of the invention.
Embodiment 1
For the present embodiment using mung bean flour as carbon source, calcium chloride is activator, and urea is that nitrogen source prepares nitrating porous carbon materials, according to
It is secondary to proceed as follows:
1.0g mung bean flour is added in 55mL deionized water, constant temperature in 80 DEG C of water-baths is placed in and stirs, then into mixture
2.0g calcium chloride and 2.0g urea is added, constant temperature stirs 3h, is dried to obtain mixed-powder.
Reactant obtained in step (1) is placed in tube furnace, in nitrogen atmosphere, with the heating rate of 5 DEG C/min
800 DEG C are warming up to, 2h is calcined, cooled to room temperature obtains black powder.
Black powder is put into the hydrochloric acid of 1mol/L, 1.5h is stirred, stands 1~2 day, it is more up to nitrating after suction filtration is dry
Hole carbon material.
The SEM of gained nitrating mesoporous carbon sample is as shown in Figure 1, gained sample is the blocky carbon materials for containing a large amount of pore structures
Material.The nitrogen adsorption desorption curve of the sample is as shown in Fig. 2, curve shows the hysteresis loop of mesoporous material in figure, the ratio tested out
Surface area is up to 994.61m2/g.In 6M KOH electrolyte, the specific capacitance of the sample, such as Fig. 3 are tested using cyclic voltammetry
Shown, under the sweep speed of 50mv/s, specific capacitance is up to 246.20F/g.
Embodiment 2
For the present embodiment using mung bean flour as carbon source, calcium chloride is activator, and urea is that nitrogen source prepares nitrating porous carbon materials, according to
It is secondary to proceed as follows:
(1) 1.0g mung bean flour is added in 55mL deionized water, is placed in 80 DEG C of water-baths constant temperature and stirs, then toward mixture
Middle addition 1.0g calcium chloride and 1.0g urea, constant temperature stir 0.5h, are dried to obtain mixed-powder.
(2) mixed-powder obtained in step (1) is placed in tube furnace, in nitrogen atmosphere, with the heating of 5 DEG C/min
Rate is warming up to 700 DEG C, calcines 2h, and cooled to room temperature obtains black powder.
(3) black powder is put into the hydrochloric acid of 0.5mol/L, stirs 1.5h, stand 1~2 day, after suction filtration is dry to obtain the final product
Nitrating porous carbon materials.
The SEM of gained nitrating mesoporous carbon sample is as shown in figure 4, gained sample is the blocky carbon materials for containing a large amount of pore structures
Material.The nitrogen adsorption desorption curve of the sample is as shown in figure 5, curve shows the hysteresis loop of mesoporous material in figure, the ratio tested out
Surface area is up to 859.32m2/g.In 6M KOH electrolyte, the specific capacitance of the sample, such as Fig. 3 are tested using cyclic voltammetry
Shown, under the sweep speed of 50mv/s, specific capacitance is up to 79.67F/g.
Embodiment 3
For the present embodiment using mung bean flour as carbon source, calcium chloride is activator, and urea is that nitrogen source prepares nitrating porous carbon materials, according to
It is secondary to proceed as follows:
(1) 1.0g mung bean flour is added in 55mL deionized water, is placed in 80 DEG C of water-baths constant temperature and stirs, then toward mixture
Middle addition 4.0g calcium chloride and 2.0g urea, constant temperature stir 2h, are dried to obtain mixed-powder.
(2) mixed-powder obtained in step (1) is placed in tube furnace, in nitrogen atmosphere, with the heating of 5 DEG C/min
Rate is warming up to 900 DEG C, calcines 2h, and cooled to room temperature obtains black powder.
(3) black powder is put into the hydrochloric acid of 2mol/L, stirs 1.5h, stand 1~2 day, mixed to obtain the final product after filtering drying
Nitrogen porous carbon materials.
In 6M KOH electrolyte, the specific capacitance of the sample is tested using cyclic voltammetry, as shown in figure 3, in 50mv/s
Sweep speed under, specific capacitance is up to 165F/g.
Embodiment 4
For the present embodiment using mung bean as carbon source, calcium chloride is activator, and urea is that nitrogen source prepares nitrating porous carbon materials, successively
It proceeds as follows:
1.0g mung bean flour is added in 55mL deionized water, constant temperature in 80 DEG C of water-baths is placed in and stirs, then into mixture
2.0g calcium chloride and 3.0g urea is added, constant temperature stirs 1h, is dried to obtain mixed-powder.
Mixed-powder obtained in step (1) is placed in tube furnace, in nitrogen atmosphere, with the heating speed of 5 DEG C/min
Rate is warming up to 800 DEG C, calcines 2h, and cooled to room temperature obtains black powder.
Black powder is put into the hydrochloric acid of 1mol/L, 1.5h is stirred, stands 1~2 day, it is more up to nitrating after suction filtration is dry
Hole carbon material.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and
Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and
Modification, all should be contained within the scope of the invention.
Claims (10)
1. a kind of preparation method of nitrating porous carbon, which comprises the following steps:
S1: mung bean flour is added to the water, and after mixing evenly, adds activator and urea obtains mixed liquor；
S2: the mixed liquor that S1 is obtained is stirred, and sufficiently after reaction, re-dry obtains reactant；
S3: reactant obtained in S2 is calcined under atmosphere of inert gases, sour processing is carried out after calcining again, obtains nitrating
Porous carbon.
2. the preparation method of nitrating porous carbon according to claim 1, which is characterized in that in S3, after the completion of acid processing
It also successively include suction filtration, washing and drying steps.
3. the preparation method of nitrating porous carbon according to claim 1, which is characterized in that in S1, the activator is
Calcium chloride.
4. the preparation method of nitrating porous carbon according to claim 1, which is characterized in that in S1, stirring condition setting
Are as follows: whipping temp is 80 DEG C, and mixing time is 0.5~3h.
5. the preparation method of nitrating porous carbon according to claim 1, which is characterized in that in S1, the mung bean flour with
The mass ratio of the activator is 1:(1~4).
6. the preparation method of nitrating porous carbon according to claim 1, which is characterized in that in S1, the mung bean flour with
The mass ratio of the urea is 1:(1~3).
7. the preparation method of nitrating porous carbon according to claim 1, which is characterized in that in S3, the journey of the calcining
Sequence setting are as follows: be warming up to 700~900 DEG C with the heating rate of 5 DEG C/min.
8. the preparation method of nitrating porous carbon according to claim 1, which is characterized in that in S3, the acid processing
Process are as follows: use inorganic acid pickling at normal temperature；The inorganic acid is one of hydrochloric acid, nitric acid, sulfuric acid or any combination thereof；
The concentration of the inorganic acid is 0.5-2mol/L.
9. the nitrating porous carbon that any one of -8 the methods are prepared according to claim 1.
10. application of the nitrating porous carbon according to claim 9 in electrochemical field.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110841595A (en) * | 2019-12-02 | 2020-02-28 | 国网江苏省电力有限公司电力科学研究院 | Preparation method and application of nitrogen-doped graphitized carbon material |
| CN112299389A (en) * | 2020-09-23 | 2021-02-02 | 鸡西市唯大新材料科技有限公司 | Method for preparing sodium ion carbon negative electrode material by using nitrogen-doped porous biomass carbon |
-
2018
- 2018-11-08 CN CN201811325564.7A patent/CN109573976A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110841595A (en) * | 2019-12-02 | 2020-02-28 | 国网江苏省电力有限公司电力科学研究院 | Preparation method and application of nitrogen-doped graphitized carbon material |
| CN112299389A (en) * | 2020-09-23 | 2021-02-02 | 鸡西市唯大新材料科技有限公司 | Method for preparing sodium ion carbon negative electrode material by using nitrogen-doped porous biomass carbon |
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