CN106672935A - Preparation method of nitrogen-doped hollow porous carbon - Google Patents
Preparation method of nitrogen-doped hollow porous carbon Download PDFInfo
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- CN106672935A CN106672935A CN201611213497.0A CN201611213497A CN106672935A CN 106672935 A CN106672935 A CN 106672935A CN 201611213497 A CN201611213497 A CN 201611213497A CN 106672935 A CN106672935 A CN 106672935A
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
Abstract
The invention relates to a preparation method of nitrogen-doped porous carbon. The preparation method specifically comprises the following steps of firstly, preparing a manganese dioxide precursor, preparing a mixing solution containing a certain ratio of aniline and pyrrole monomers, dispersing a manganese dioxide powder into the mixing solution, cooling the dispersing liquid to the temperature below 10 DEG C, adding an acid solution into the dispersing liquid, reacting for a period of time at low temperature, and separating, so as to obtain a product; finally, carbonizing at high temperature under the protection atmosphere, so as to obtain the nitrogen-doped hollow porous carbon material. The preparation method has the characteristics that the synthesis technology is simple, the safe, green and pollution-free effects are realized in the synthesis process, the byproducts can be recycled, the preparation method is suitable for industrial production, and the like; the property of the nitrogen-doped porous carbon is excellent, the specific surface area is higher, and the nitrogen-doped porous carbon can be widely applied to the fields of energy storage, catalysis, adsorption, such as supercapacitors.
Description
Technical field
The invention belongs to porous material preparation field, and in particular to a kind of preparation side of the hollow porous carbon materials of N doping
Method.
Background technology
Recent years, porous carbon materials are because have such as high electric conductivity, big specific surface area, cheap price etc. excellent
Point, has attracted the attention of increasing researcher, has obtained more and more widely studying, and is widely used as ultracapacitor
Electrode material, the negative material of lithium ion battery, gas adsorption material and catalyst carrier material etc., and there is hollow structure
Nitrogen-doped porous carbon material because have macropore (>50nm), mesoporous (2-50nm), micropore (<Complete pore system 2nm),
The needs that can be competent under different application field, while the presence of nitrogen-atoms can significantly improve the electrochemistry of material after N doping
Performance and hydrophilic, therefore with wide market prospect.As the hollow N doping porous carbon that can be used with industrialization promotion
Material, first has to ensure that prepared porous carbon materials have suitable pore-size distribution and higher specific surface area, secondly asks a price
Lattice are cheap, and building-up process is pollution-free, environmentally friendly, it is therefore desirable to accomplish that synthesising by-product can be with recycling.
Current some porous carbon materials of commercial applications, because itself irrational pore-size distribution and complicated tediously long and right
The disagreeableness building-up process of environment, is also not reaching to above-mentioned requirements.Such as electrode material for super capacitor, for ultracapacitor
For, existing electrode material, such as Chinese patent 201610272051.9 need special reaction raw materials as not yet realized industry
Change the graphene oxide and ionic liquid of volume production, and need activation to use, other some patents, such as Chinese patent
201410705947.2, it is also desirable to which loose structure can just be obtained by activated material under alkaline matter high temperature, but alkaline matter
High temperature etching can damage reaction vessel, and building-up process also can be impacted to environment.Almost China without this area
Patent is related to the recycling of synthetic product side-product.Therefore, a kind of suitable pore-size distribution and higher of having concurrently is found
Specific surface area and and into process is pollution-free, synthesising by-product recoverable and cheap porous carbon materials synthetic method
With very great meaning.
The content of the invention
The technical problem to be solved
In order to avoid the deficiencies in the prior art part, the present invention proposes a kind of preparation side of the hollow porous carbon materials of N doping
Method, it is not necessary to tediously long activation and template removal step, can obtain the higher N doping of specific surface area hollow by direct carbonization
Porous carbon materials, and the method is raw materials used cheap, it is easy to prepare, building-up process is environmentally friendly.
Technical scheme
The preparation method of the hollow porous carbon materials of a kind of N doping, it is characterised in that step is as follows:
Step 1:Manganese dioxide precursor powder is scattered in the mixed solution of aniline and pyrrole monomer, is disperseed
Liquid;The aniline is 0.5 with the mol ratio of pyrrole monomer:1-2:1;The manganese dioxide and aniline and the mol ratio of pyrrole monomer
Example is 0.01:1-2000:1;
Step 2:Dispersion liquid is cooled to into less than 10 DEG C, acid solution is added, in a low temperature of 0-10 DEG C, 1-24 is little for reaction
When after separating obtained product;It is 0.5 that the acid solution of the addition causes hydrion and the mol ratio of manganese dioxide in solution:100-
4:100;
Step 3:The high temperature cabonization under protective atmosphere, obtains the hollow porous carbon materials of N doping;The pyrocarbon chemical industry
Heating rate is 0.1-20 DEG C/min in skill, and temperature is 600-1200 DEG C, and carbonization time is 2-20 hours;The protective atmosphere
For nitrogen, argon or helium.
The manganese dioxide precursor construction be one-dimensional nano line, nanotube, nanometer rods, two-dimensional nano piece, three-dimensional manometer
Flower or Hemicentrotus seu Strongylocentrotuss shape nanosphere pattern.
The manganese dioxide presoma is prepared by hydro-thermal method, chemical precipitation method or electrochemical deposition method.
The aniline is 1 with the mol ratio of pyrrole monomer:1.
The manganese dioxide is 1000 with the molar ratio of aniline and pyrrole monomer:1-600:1.
The acid solution is sulphuric acid, hydrochloric acid, nitric acid or acetic acid etc., and solution concentration is 0.01-5mol/L.
The step 2 dispersion liquid cold rnning enters after acid solution in a low temperature of 0-5 DEG C, reacts 6-8 hours.
Beneficial effect
A kind of preparation method of the hollow porous carbon materials of N doping proposed by the present invention, principle is as follows.Aniline and pyrroles are complete
After CL, because pyrroles is hydrophobic, aniline is hydrophilic, and pyrroles can be gathered in around manganese dioxide surface, and aniline then disperses in water
Open.After adding acid, under acid effect, manganese dioxide reacts with aniline, pyrroles, and aniline and pyrroles are copolymerized, in dioxy
Changing the aniline and pyrrole concentrations formed around manganese near copolymer, manganese dioxide in solution reduces, unreacted aniline in solution
Can diffuse through to come with pyrroles, reaction is persistently carried out.Simultaneously manganese dioxide is consumed as oxidant, generates divalent manganesetion,
Aniline and pyrroles ultimately form hollow copolymer.Because the copolymer has solid carbon skeleton network, therefore in higher temperature
It is carbonized under degree and harsher Carbonization Conditions and still can keep pore structure and do not cave in, it is possible to is directly obtained by carbonization
Loose structure.
Beneficial effects of the present invention are as follows.First, raw material used in the present invention is all common and cheap raw material,
Mature production technology.Secondly, the whole synthesis technique of the present invention does not have huge using to Fluohydric acid., surfactant etc. to environment
Big harm has the reagent of serious harm to the person, equipment.Again, the filtrate obtained by step (3) of the invention obtains after being evaporated
Manganese sulfate can be used for step (1) synthesis manganese dioxide just, can be recycled, also apply be applicable to other field, meet current
The theme economized on resources with environmental protection, and eliminate harm of the metal ion to environment, it is not necessary to other means back and forth
Purification waste liquid is received, environmental benefit is obvious.In addition, by the pattern of control manganese dioxide presoma, thus it is possible to vary final to produce
The pattern of thing porous carbon materials.Simple, the prepared porous carbon excellent performance of last synthesis technique of the present invention, is adapted to industry metaplasia
Produce.
Description of the drawings
Fig. 1 is the electron scanning micrograph of manganese dioxide nano pipe prepared by embodiment 1.
Fig. 2 is the electron scanning micrograph of the intermediate product prepared by embodiment 1.
Fig. 3 is the electron scanning micrograph of the final product N doping porous carbon prepared by embodiment 1.
Fig. 4 is the nitrogen adsorption desorption test curve of the N doping porous carbon prepared by embodiment 1.
Fig. 5 is the electron scanning micrograph of the three-dimensional manganese dioxide prepared by embodiment 2.
Fig. 6 is the electron scanning micrograph of the three-dimensional nitrogen-doped porous carbon material prepared by embodiment 2.
Nitrogen-doped porous carbon materials of the Fig. 7 prepared by embodiment 4 is when as electrode material for super capacitor not
With the cyclic voltammetry curve under sweep speed.
Specific embodiment
In conjunction with embodiment, accompanying drawing, the invention will be further described:
Embodiment 1
Take 0.7g KMnO4, 1.4g MnSO4, in being dissolved in 70ml water.Solution is poured in water heating kettle, at 150 DEG C 12 are incubated
Hour, after it is cooled to room temperature, filtering and washing products therefrom and the desciccate at 60 DEG C.The brown ceramic powder for now obtaining is i.e.
The manganese dioxide nano pipe shown in accompanying drawing 1.
Prepared manganese dioxide nano pipe 400mg, aniline 0.152ml, pyrroles 0.116ml is taken, in adding 180ml water,
After stirring 20min, solution is put into into freezing 30min in refrigerator (3-5 DEG C), 1ml H are added after taking-up2SO4, 0.5min is stirred, put
Enter (3-5 DEG C) reaction 8h in refrigerator, by product sucking filtration to filtrate in neutrality, be dried at 60 DEG C.The black product for now obtaining
Intermediate product as shown in accompanying drawing 2.
Intermediate product 400mg is taken, in being placed in tube furnace, in a nitrogen atmosphere, with 5 DEG C/min ramps to 900 DEG C, is protected
Warm 7h, naturally cools to afterwards room temperature.The product for now obtaining is the nitrogen-doped porous carbon material shown in accompanying drawing 3.
Jing nitrogen adsorption desorption is tested, and the specific surface area of products therefrom is 538m2/ g, pore volume is 1.2cm3/g.
Embodiment 2
Take 0.7g KMnO4, 1.5g MnSO4, in being dissolved in 70ml water.Solution is poured in water heating kettle, insulation 5 is little at 120 DEG C
When, after it is cooled to room temperature, filtering and washing products therefrom and the desciccate at 60 DEG C.Now obtain three-dimensional shown in accompanying drawing 5
Manganese dioxide.
Prepared manganese dioxide 200mg, aniline 0.38ml, pyrroles 0.29ml is taken, in adding 60ml water, 20min is stirred
Afterwards, solution is put into into freezing 30min in refrigerator (3-5 DEG C), adds the 15ml for freezing in advance to contain the dense H of 1ml after taking-up2SO4's
Aqueous solution, stirs 0.5min, is put in refrigerator (3-5 DEG C) reaction 8h, by product sucking filtration to filtrate in neutrality, does at 60 DEG C
It is dry, obtain intermediate product.
Intermediate product 200mg is taken, in being placed in tube furnace, in a nitrogen atmosphere, with 5 DEG C/min ramps to 900 DEG C, is protected
Warm 7h, naturally cools to afterwards room temperature.The product for now obtaining is the nitrogen-doped porous carbon material shown in accompanying drawing 6.
Embodiment 3
Take 0.7g KMnO4, 1.5g MnSO4, in being dissolved in 70ml water.Solution is poured in water heating kettle, at 160 DEG C 12 are incubated
Hour, after it is cooled to room temperature, filtering and washing products therefrom and the desciccate at 60 DEG C.Now obtain 1-dimention nano wire
Manganese dioxide.
Prepared manganese dioxide 400mg, aniline 0.38ml, pyrroles 0.29ml is taken, in adding 60ml water, 20min is stirred
Afterwards, solution is put into into freezing 30min in refrigerator (3-5 DEG C), adds the 15ml for freezing in advance to contain 2ml H after taking-up2SO4's
Aqueous solution, stirs 0.5min, is put in refrigerator (3-5 DEG C) reaction 8h, by product sucking filtration to filtrate in neutrality, does at 60 DEG C
It is dry, obtain intermediate product.
Intermediate product 200mg is taken, in being placed in tube furnace, in a nitrogen atmosphere, with 5 DEG C/min ramps to 900 DEG C, is protected
Warm 15h, naturally cools to afterwards room temperature.Now obtain one-dimensional nitrogen-doped porous carbon material.Its nitrogen adsorption desorption test result is such as
Shown in accompanying drawing 7, specific surface area is 720m2/g。
Embodiment 4
Take 0.7g KMnO4, 1.5g MnSO4, in being dissolved in 70ml water.Solution is poured in water heating kettle, at 150 DEG C 10 are incubated
Hour, after it is cooled to room temperature, filtering and washing products therefrom and the desciccate at 60 DEG C.
Prepared manganese dioxide nano pipe 400mg, aniline 0.38ml, pyrroles 0.29ml is taken, in adding 60ml water, stirring
After 20min, solution is put into into freezing 30min in refrigerator (3-5 DEG C), 1ml H are added after taking-up2SO4, 0.5min is stirred, it is put into ice
(3-5 DEG C) reaction 8h in case, by product sucking filtration to filtrate in neutrality, is dried at 60 DEG C.
Intermediate product 400mg is taken, in being placed in tube furnace, in a nitrogen atmosphere, with 5 DEG C/min ramps to 900 DEG C, is protected
Warm 10h, naturally cools to afterwards room temperature.
Potassium hydroxide solution with 6M carries out capacitive property survey more using three-electrode system as electrolyte to the materials for preparing
Examination.Cyclic voltammetry curve of the products therefrom under different scanning rates shows that the high rate performance of product is excellent, and products therefrom is in 1A/
Capacity is 209F/g under the electric current density of g, and capability retention is 100% Jing after 5000 circulations under 50A/g, electrochemical impedance
Spectrum shows the resistance very little of material, simultaneously as material has excellent multiplying power property, so material can carry out high-power filling
Electric discharge, is suitable as the electrode material of ultracapacitor.
Claims (7)
1. the preparation method of the hollow porous carbon materials of a kind of N doping, it is characterised in that step is as follows:
Step 1:Manganese dioxide precursor powder is scattered in the mixed solution of aniline and pyrrole monomer, dispersion liquid is obtained;Institute
It is 0.5 that aniline is stated with the mol ratio of pyrrole monomer:1-2:1;The manganese dioxide is with the molar ratio of aniline and pyrrole monomer
0.01:1-2000:1;
Step 2:Dispersion liquid is cooled to into less than 10 DEG C, acid solution is added, in a low temperature of 0-10 DEG C, after reaction 1-24 hours
Separating obtained product;It is 0.5 that the acid solution of the addition causes hydrion and the mol ratio of manganese dioxide in solution:100-4:
100;
Step 3:The high temperature cabonization under protective atmosphere, obtains the hollow porous carbon materials of N doping;In the high temperature cabonization technique
Heating rate is 0.1-20 DEG C/min, and temperature is 600-1200 DEG C, and carbonization time is 2-20 hours;The protective atmosphere is nitrogen
Gas, argon or helium.
2. the preparation method of the hollow porous carbon materials of N doping according to claim 1, it is characterised in that:The manganese dioxide
Precursor construction is one-dimensional nano line, nanotube, nanometer rods, and two-dimensional nano piece, three-dimensional manometer is spent or Hemicentrotus seu Strongylocentrotuss shape nanosphere pattern.
3. the preparation method of the hollow porous carbon materials of N doping according to claim 1 or claim 2, it is characterised in that:The dioxy
Change manganese presoma to prepare by hydro-thermal method, chemical precipitation method or electrochemical deposition method.
4. the preparation method of the hollow porous carbon materials of N doping according to claim 1, it is characterised in that:The aniline and pyrrole
The mol ratio for coughing up monomer is 1:1.
5. the preparation method of the hollow porous carbon materials of N doping according to claim 1, it is characterised in that:The manganese dioxide
It is 1000 with the molar ratio of aniline and pyrrole monomer:1-600:1.
6. the preparation method of the hollow porous carbon materials of N doping according to claim 1, it is characterised in that:The acid solution is
Sulphuric acid, hydrochloric acid, nitric acid or acetic acid etc., solution concentration is 0.01-5mol/L.
7. the preparation method of the hollow porous carbon materials of N doping according to claim 1, it is characterised in that:The step 2 point
Dispersion liquid cold rnning enters after acid solution in a low temperature of 0-5 DEG C, reacts 6-8 hours.
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Cited By (7)
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CN107706405A (en) * | 2017-11-23 | 2018-02-16 | 齐鲁工业大学 | A kind of method for preparing nitrogen or the bar-shaped Zinc ion battery positive electrode of nitrogen sulfur doping carbon coating manganese dioxide composite Nano |
CN109167074A (en) * | 2018-08-08 | 2019-01-08 | 东华大学 | The nitrogen-doped carbon nanocomposite of hollow additive Mn cobalt oxide nickel coated and preparation |
CN110451465A (en) * | 2019-09-09 | 2019-11-15 | 吉林大学 | A kind of sea urchin shape boron nitride nanometer ball-nanotube hierarchical structure and preparation method thereof |
CN110534716A (en) * | 2019-08-30 | 2019-12-03 | 华北电力大学 | A kind of porous oxidation manganese micron ball and its preparation method and application |
CN111268668A (en) * | 2020-02-17 | 2020-06-12 | 西安交通大学 | Nitrogen-doped porous nano carbon material, preparation method and application of nitrogen-doped porous nano carbon material as negative electrode material of lithium ion battery |
CN111547705A (en) * | 2020-05-12 | 2020-08-18 | 中国计量大学 | Preparation method of porous carbon electrode material |
CN114068935A (en) * | 2021-11-15 | 2022-02-18 | 大连理工大学 | High-activity Mn/Co-N double-site doped carbon material catalyst, preparation method and application thereof in lithium-sulfur battery |
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CN110534716B (en) * | 2019-08-30 | 2020-08-14 | 华北电力大学 | Porous manganese oxide micro-sphere and preparation method and application thereof |
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CN111547705A (en) * | 2020-05-12 | 2020-08-18 | 中国计量大学 | Preparation method of porous carbon electrode material |
CN111547705B (en) * | 2020-05-12 | 2022-03-29 | 中国计量大学 | Preparation method of porous carbon electrode material |
CN114068935A (en) * | 2021-11-15 | 2022-02-18 | 大连理工大学 | High-activity Mn/Co-N double-site doped carbon material catalyst, preparation method and application thereof in lithium-sulfur battery |
CN114068935B (en) * | 2021-11-15 | 2023-01-24 | 大连理工大学 | High-activity Mn/Co-N dual-site doped carbon material catalyst, preparation method and application thereof in lithium-sulfur battery |
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