CN109133030A - A kind of preparation method and applications of nitrogen-doped porous carbon material - Google Patents
A kind of preparation method and applications of nitrogen-doped porous carbon material Download PDFInfo
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- CN109133030A CN109133030A CN201811114757.8A CN201811114757A CN109133030A CN 109133030 A CN109133030 A CN 109133030A CN 201811114757 A CN201811114757 A CN 201811114757A CN 109133030 A CN109133030 A CN 109133030A
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- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a kind of preparation method and applications of nitrogen-doped porous carbon material, its preparation step includes: step 1: glucose and nitrogenous compound are add to deionized water, it is put into the carburizing reagent under certain temperature and time in autoclave after mixing evenly, using filter, washs, be dried to obtain nitrogenous precursor；Step 2: nitrogenous precursor and alkali inorganic substance being mixed, agitated, dry, calcining, activation obtain nitrogen-doped porous carbon material；Step 3: by obtained nitrogen-doped porous carbon material by washing, filtering, dry, grind up to nitrogen-doped porous carbon material, the specific surface area range of the material is in 1343-1947m2g‑1, pore-size distribution is uniform, pore-size distribution 1-2nm.The material is applied to electrode material for super capacitor and is assembled into supercapacitor, when current density is 0.5Ag‑1When, specific capacitance value is 320-423F g‑1.It has broad application prospects in fields such as supercapacitor, lithium ion batteries.
Description
Technical field
The present invention relates to porous material technical fields, and in particular to a kind of preparation method of nitrogen-doped porous carbon material and its
Using.
Background technique
Supercapacitor with power density height, has extended cycle life, charge and discharge as a kind of new and effective energy storage device
High-efficient, non-maintaining, energy conservation and environmental protection etc. series of advantages, rapidly in electric car, electric power, railway, consumer electrical product
Etc. various fields be applied.Wherein electrode material is the important component of supercapacitor, specifically include that carbon-based material,
Metal oxide (such as MnO2, NiO) and conducting polymer.Carbon electrode material has excellent electrical property, good physico
Learn stability, the advantages that high specific surface area, wherein the porous carbon materials in carbon-based material are that current application is most widely a kind of
Electrode material, since with good physical and chemical performance, such as large specific surface area, pore structure is controllable, chemical property is stable, high
The features such as thermally conductive, high conductivity and abundant raw material.
It is directed to pure carbon material, the introducing hetero-atoms such as nitrogen-atoms in porous carbon materials can be improved the profit of material surface
Moist and stability, meanwhile, reversible redox reaction can occur with electrolyte to provide fake capacitance.Therefore, nitrogen is mixed
Miscellaneous porous carbon has high specific surface area, pore structure abundant and a large amount of surface nitrogen-containing functional group, to assign the material
The properties such as unique machinery, electronics, energy storage, make it be widely used in the electrode material of supercapacitor.
However, the supercapacitor carbon compound based on pure carbon material has lower specific capacitance and energy density
(5-8WHKg-1), limit their practical application.In order to which the energy of further satisfaction modern supercapacitors rapid growth needs
It asks.Research shows that [Journal of Colloid and Interface Science 523 (2018) 133-143], nitrogen and
The hetero atoms such as oxygen doping can substantially improve electrode performance with pseudo-capacitance is introduced by the electron donor's characteristic to cut material.
In conclusion being carried out rationally while exploitation high-specific surface area nitrogen-doped porous carbon material to the distribution of its aperture structure
Control is to improve the key technology of the energy density and power density of supercapacitor.Anti-form-1,2- cyclohexanediaminetetraacetic acid are certainly
Body is rich in Dan Yang functional group, may be used as a kind of novel nitrogen source, and after incorporation anti-form-1,2- cyclohexanediaminetetraacetic acid, makes
The specific capacitance of supercapacitor is greatly improved, specific surface area with higher, the electrode material as supercapacitor
Material has very big prospect.
Summary of the invention
Adjustable aperture, high-specific surface area, the performance for promoting supercapacitor are able to achieve it is an object of the invention to provide a kind of
Meanwhile the preparation method and applications of the nitrogen-doped porous carbon material of electrode material production cost can be reduced.
In order to achieve the above-mentioned object of the invention, technical solution of the present invention is using glucose as carbon source, with anti-form-1,2- cyclohexyl diamine
Tetraacethyl is nitrogen source, uses alkali inorganic substance for activator, and stable three-dimensional porous carbon material is synthesized using chemical activation method.Benefit
Dan Yang functional group, during high temperature cabonization, such Dan Yang functional group meeting are rich in anti-form-1,2- cyclohexanediaminetetraacetic acid itself
Decompose, be conducive to the generation of carbon material pore structure, microcellular structure can be widened, increase mesoporous content, improve electrolyte from
The transmission rate of son, optimizes the high rate performance of electrode material.The pore-size distribution of carbon material is adjusted using activator, improves carbon material
Nitrogen content and electric conductivity, thus as far as possible increase material specific surface area, form the electric double layer of large area, improve super electricity
The performance of container.
Realizing the specific technical solution of the object of the invention is:
A kind of preparation method of nitrogen-doped porous carbon material, it is anti-through hydro-thermal by certain mass ratio with nitrogenous compound by glucose
It answers, is prepared using alkali inorganic substance calcining and activating.Its preparation includes the following steps:
Step 1: glucose and nitrogenous compound being added in a certain amount of deionized water by certain mass ratio, after mixing evenly
It is put into autoclave, carbonizationization is answered under certain temperature and time, is refiltered, washs, is dried to obtain nitrogenous precursor；
Step 2: step 1 gained nitrogenous precursor and alkali inorganic substance are impregnated by certain mass than mixing in deionized water
Afterwards, it is put into after drying in atmosphere furnace under nitrogen protection, activates to obtain nitrogen-doped modified porous carbon with certain calcination condition
Material；
Step 3: above-mentioned product being impregnated with hydrochloric acid solution, obtains nitrogen-doped porous carbon by washing, filtering, drying, grinding
Material.
The glucose of the step 1 and the mass ratio of nitrogenous compound are 4.0: 0.5-4.0, and hydrothermal temperature is
120-200 DEG C, reaction time 4-10h.
The nitrogenous compound of the step 1 includes anti-form-1,2- cyclohexanediaminetetraacetic acid, and the alkali inorganic substance is hydrogen
Potassium oxide, sodium hydroxide, potassium carbonate or zinc chloride.
The nitrogenous compound of the step 2 and the mass ratio of alkali inorganic substance are 1.0: 1.0-4.0.
It is 600-800 DEG C that the calcining and activating condition of the step 2, which is activation temperature, activation time 2-5h.
A kind of nitrogen-doped porous carbon material realized according to the above method, through scanning electron microscope test, the results showed that, it should
Carbon material is cellular porous structure.It is tested through adsorption isothermal curve and pore-size distribution, specific surface area 1343-1947
m2g-1, pore-size distribution 1-2nm.
Using a kind of above-mentioned nitrogen-doped porous carbon material as the application of electrode material for super capacitor, super capacitor is made
Device, through chronoptentiometry test result, when current density is 0.5 A g-1When, specific capacitance value is in 320-423F g-1.Through recycling
Volt-ampere test, under different sweep speeds, cyclic voltammetry curve keeps good and is similar to rectangular shape, shows to have good
The performance of electric double layer capacitance.
The advantages and positive effects of the present invention are:
(1) anti-form-1, the 2- ring of Dan Yang functional group are rich in the preparation method of nitrogen-doped porous carbon material of the present invention using itself
Ethylenediamine tetraacetic acid (EDTA) is nitrogen source, decomposes in the condition of high temperature and advantageously forms more micropores, increases the ratio table of carbon material
Area, and different types of nitrogen-atoms can be mixed on carbon wall, more electric double layer capacitances and counterfeit electricity are provided for supercapacitor
Hold；
(2) it uses alkali inorganic substance for activator in the preparation method of nitrogen-doped porous carbon material of the present invention, utilizes chemical activation
Method increases the specific surface area of carbon material, synthesizes more stable three-dimensional porous carbon material.
(3) preparation condition of nitrogen-doped porous carbon material of the present invention is mild, and low energy consumption, and simple process is feasible, reduces more
Hole carbon material preparation cost.
(4) specific surface area of N doping porous structure carbon material prepared by the present invention is 1343-1947m2g-1, average pore size
The performance of the double layer capacitor of supercapacitor is improved for 1-2nm；Using making electrode material for super capacitor, mesoporous is
The transmission channel of electrolyte ion, macroporous structure can play the role of electrolyte buffer pool, realize electrode of super capacitor
Good high rate performance, and there is good cyclical stability, when current density is 0.5Ag-1When, specific capacitance value range 320 ~
423Fg-1。
Detailed description of the invention:
Fig. 1 is the scanning electron microscopy picture figure of nitrogen-doped porous carbon material；
Fig. 2 is the low temperature nitrogen adsorption isothermal curve of nitrogen-doped porous carbon material；
Fig. 3 is the pore size distribution curve of nitrogen-doped porous carbon material；
Fig. 4 is charge-discharge performance curve of the nitrogen-doped porous carbon material in different current densities；
Fig. 5 is the capacitor cyclic voltammogram of nitrogen-doped porous carbon material.
Specific embodiment
The present invention is described in further detail the content of present invention in conjunction with Figure of description, but be not pair by embodiment
Limitation of the invention.
Embodiment 1
A kind of preparation of nitrogen-doped porous carbon material, method and step are as follows:
4g glucose and 2g anti-form-1,2- cyclohexanediaminetetraacetic acid are added separately in deionized water by step 1), are stirred evenly
After be put into 180 DEG C of reaction 6h in autoclave, be filtered, washed, be dried to obtain nitrogenous precursor；
Nitrogenous precursor obtained by step 1) and alkali inorganic substance KOH are that 1.0:2.0 is mixed by step 2 in mass ratio, in deionization
It stirs evenly in water, is put into tube furnace after drying, calcining and activating temperature is 700 DEG C under nitrogen atmosphere protection, activation time
Nitrogen-doped modified porous carbon materials are obtained for 3h；
Step 3) impregnates above-mentioned product 1M HCl solution, and is filtered, washed to neutrality with deionized water, grinds after drying,
Obtain nitrogen-doped porous carbon material.
It, as a result as shown in Figure 1, should by the nitrogen-doped porous carbon material prepared in embodiment through scanning electron microscope test
Carbon material shows cellular porous structure.
The nitrogen-doped porous carbon material prepared in embodiment is tested through adsorption isothermal curve and pore-size distribution, as a result as schemed
Shown in 2 and 3, the results show that its specific surface area with higher, reaches 1947m2g-1, a large amount of micropore and suitable mesoporous, put down
Equal aperture is 1.36nm.
Using the nitrogen-doped porous carbon material prepared in embodiment as electrode material for super capacitor in application, constant current fills
Discharge test is as shown in figure 4, when current density is 0.5 Ag-1When, specific capacitance value reaches 423Fg-1。
Using the nitrogen-doped porous carbon material prepared in embodiment as electrode material for super capacitor in application, cyclic voltammetric
Test results are shown in figure 5, and under different sweep speeds, cyclic voltammetry curve keeps good and is similar to rectangular shape, table
The bright performance for having good electric double layer capacitance.
Embodiment 2
A kind of preparation of nitrogen-doped porous carbon material, method and step are as follows:
Step 1: 4g glucose and 1g anti-form-1,2- cyclohexanediaminetetraacetic acid being added separately in deionized water, stirred evenly
After be put into 120 DEG C of reaction 10h in autoclave, be filtered, washed, be dried to obtain nitrogenous precursor；
Step 2: being in mass ratio that 1.0:4.0 is mixed by nitrogenous precursor obtained by step 1) and alkali inorganic substance, in deionized water
In stir evenly, be put into tube furnace after drying, under nitrogen protection calcining and activating temperature be 800 DEG C, activation time 4h is obtained
To nitrogen-doped modified porous carbon materials；
Step 3) impregnates above-mentioned product 1M HCl solution, and is filtered, washed to neutrality with deionized water, grinds after drying,
Obtain nitrogen-doped porous carbon material.
Obtained porous carbon materials are agraphitic carbon through XRD test, and SEM is porous structure, specific surface area as the result is shown
For 1342.54 m2g-1, average pore size is 3.59 nm, supercapacitor is prepared into, when current density is 0.5Ag-1, than electricity
Capacitance reaches 380Fg-1。
Embodiment 3
A kind of preparation of nitrogen-doped porous carbon material, method and step are as follows:
Step 1: 4g glucose and 2g anti-form-1,2- cyclohexanediaminetetraacetic acid being added separately in deionized water, stirred evenly
After be put into 160 DEG C of reaction 8h in autoclave, be filtered, washed, be dried to obtain nitrogenous precursor；
Step 2: being in mass ratio that 1.0:3.0 is mixed by nitrogenous precursor obtained by step 1) and alkali inorganic substance KOH, in deionization
It stirring evenly in water, is put into tube furnace after drying, calcining and activating temperature is 700 DEG C, activation time 5h under nitrogen protection,
Obtain nitrogen-doped modified porous carbon materials；
Step 3) impregnates above-mentioned product 1M HCl solution, and is filtered, washed to neutrality with deionized water, grinds after drying,
Obtain nitrogen-doped porous carbon material.
Obtained porous carbon materials are agraphitic carbon through XRD test, and SEM is porous structure, specific surface area as the result is shown
For 1742.54m2 g-1, it is 0.5Ag in current density that average pore size 2.38nm, which is prepared into supercapacitor,-1When, specific capacitance
Value reaches 398Fg-1。
Embodiment 4
A kind of preparation of nitrogen-doped porous carbon material, method and step are as follows:
Step 1: 4g glucose and 3g anti-form-1,2- cyclohexanediaminetetraacetic acid being added separately in deionized water, stirred evenly
After be put into 200 DEG C of reaction 4h in autoclave, be filtered, washed, be dried to obtain nitrogenous precursor；
Step 2: being in mass ratio that 1.0:1.0 is mixed by nitrogenous precursor obtained by step 1) and alkali inorganic substance KOH, in deionization
It stirring evenly in water, is put into tube furnace after drying, calcining and activating temperature is 600 DEG C, activation time 5h under nitrogen protection,
Obtain nitrogen-doped modified porous carbon materials；
Step 3) impregnates above-mentioned product 1M HCl solution, and is filtered, washed to neutrality with deionized water, grinds after drying,
Obtain nitrogen-doped porous carbon material.
Obtained porous carbon materials are agraphitic carbon through XRD test, and SEM is porous structure, specific surface area as the result is shown
For 1845.32 m2g-1, it is 0.5Ag in current density that average pore size 3.21nm, which is prepared into supercapacitor,-1When, specific capacitance
Value reaches 395Fg-1。
Claims (6)
1. a kind of preparation method of nitrogen-doped porous carbon material, it is characterised in that: press certain matter by glucose and nitrogenous compound
Ratio is measured through hydro-thermal reaction, is prepared using alkali inorganic substance calcining and activating, the specific surface area of porous carbon materials is 1343-1947
m2g-1, pore-size distribution 1-2nm；Its preparation process includes the following steps:
Step 1: glucose and nitrogenous compound being added in a certain amount of deionized water by certain mass ratio, after mixing evenly
It is put into autoclave, the hydro-thermal reaction under certain temperature and time refilters, washs, is dried to obtain nitrogenous precursor；
Step 2: step 1 gained nitrogenous precursor and alkali inorganic substance are impregnated by certain mass than mixing in deionized water
Afterwards, it dries, then puts into atmosphere furnace under nitrogen protection, obtained with calcining and activating under certain condition nitrogen-doped modified porous
Carbon material crude product；
Step 3: step 2 gained porous carbon materials product 1M hydrochloric acid solution being impregnated, by washing, filtering, drying, is ground
To porous carbon materials.
2. a kind of preparation method of nitrogen-doped porous carbon material according to claim 1, it is characterised in that: described in step 1
Glucose and the mass ratio of nitrogenous compound be 4.0:0.5-4.0, hydrothermal temperature is 120-200 DEG C, and the reaction time is
4-10h。
3. a kind of preparation method of nitrogen-doped porous carbon material according to claim 1, it is characterised in that: described in step 1
Nitrogenous compound be anti-form-1,2- cyclohexanediaminetetraacetic acid.
4. a kind of preparation method of nitrogen-doped porous carbon material according to claim 1, it is characterised in that: described in step 2
Nitrogenous precursor and alkali inorganic substance mass ratio be 1.0:1.0-4.0, the alkali inorganic substance be potassium hydroxide, hydrogen-oxygen
Change sodium, potassium carbonate or zinc chloride.
5. a kind of preparation method of nitrogen-doped porous carbon material according to claim 1, it is characterised in that: described in step 2
Calcining and activating condition are as follows: activation temperature be 600-800 DEG C, activation time 2-5h.
6. application of the nitrogen-doped porous carbon material as prepared by claim 1 as electrode material for super capacitor, feature
It is: when current density is 0.5Ag-1When, specific capacitance value is 320-423Fg-1。
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| CN111909600B (en) * | 2020-08-06 | 2021-11-12 | 广东创辉鑫材科技股份有限公司 | Manufacturing method of high-thermal-conductivity resin for metal substrate |
| CN111943199A (en) * | 2020-08-21 | 2020-11-17 | 江西省科学院应用化学研究所 | Method for preparing sulfur-nitrogen co-doped porous carbon material by using potassium hydroquinone sulfate as activating agent |
| CN112736252A (en) * | 2020-12-30 | 2021-04-30 | 广州流行色服饰有限公司 | Mesoporous nickel oxide loaded nitrogen-doped porous carbon negative electrode material and preparation method thereof |
| CN113135568A (en) * | 2021-05-27 | 2021-07-20 | 吉林大学 | Nitrogen-doped porous carbon material and preparation method and application thereof |
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Application publication date: 20190104 |