CN108529621A - A kind of preparation and its application of nitrogen-doped porous carbon material - Google Patents

A kind of preparation and its application of nitrogen-doped porous carbon material Download PDF

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Publication number
CN108529621A
CN108529621A CN201810456306.6A CN201810456306A CN108529621A CN 108529621 A CN108529621 A CN 108529621A CN 201810456306 A CN201810456306 A CN 201810456306A CN 108529621 A CN108529621 A CN 108529621A
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nitrogen
carbon
porous carbon
ginkgo leaf
doped porous
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CN201810456306.6A
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Chinese (zh)
Inventor
孙立贤
李晶华
徐芬
洪先永
陈沛荣
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Guilin University of Electronic Technology
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Guilin University of Electronic Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/318Preparation characterised by the starting materials
    • C01B32/324Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/30Active carbon
    • C01B32/312Preparation
    • C01B32/342Preparation characterised by non-gaseous activating agents
    • C01B32/348Metallic compounds
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors [EDLCs]; Processes specially adapted for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their materials
    • H01G11/32Carbon-based, e.g. activated carbon materials
    • H01G11/34Carbon-based, e.g. activated carbon materials characterised by carbonisation or activation of carbon
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors [EDLCs]; Processes specially adapted for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their materials
    • H01G11/32Carbon-based, e.g. activated carbon materials
    • H01G11/44Raw materials therefor, e.g. resins or coal
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

Abstract

The invention discloses a kind of nitrogen-doped porous carbon materials, are prepared with nitrogenous compound and alkali inorganic substance calcining and activating after low-temperature carbonization is handled by ginkgo leaf, specific surface area range is in 888 ~ 1132 m2g‑1, pore-size distribution is uniform, and distribution is 1.20 ~ 2.13nm.Preparation method includes:Step 1)Ginkgo leaf low-temperature carbonization is obtained into carbon matrix precursor;Step 2)Carbon matrix precursor is subjected to activation process;Step 3)The post-processing of nitrogen-doped carbon material.As the application of electrode material for super capacitor, when current density is 1A g‑1When, specific capacitance value range is in 254 ~ 356F g‑1.It is carbon source that the present invention, which selects ginkgo leaf, improves ginkgo leaf comprehensive resource utilization rate, obtains the product of high additive value, and have good chemical property.

Description

A kind of preparation and its application of nitrogen-doped porous carbon material
Technical field
The present invention relates to porous material technical fields, and in particular to a kind of preparation and application of nitrogen-doped porous carbon material.
Background technology
Electric chemical super capacitor is a kind of novel energy storage apparatus between traditional capacitor and rechargeable battery, because of tool There is outstanding advantages of high-specific-power and long-life, has become the research hotspot in electrochemical energy storage field in recent years.Carbon material is one The electrode material of kind double layer capacitor, due to its large specific surface area, physical and chemical performance is stablized, and the conditions such as at low cost are vast Researcher is of interest.Activated carbon, template carbon, carbon nanotube, carbon aerogels, ordered mesopore carbon all become the electrode of ultracapacitor Material, and by regulating and controlling specific surface area, electric conductivity, the length in aperture and the distribution and microscopic appearance etc. of carbon material because usually Control the capacitive property of material.
Biomass carbon is to prepare porous carbon by raw material of abandoned biomass, can effectively reduce house refuse and waste is direct Burning handles discharged carbon dioxide, while obtaining the porous carbon products of high added value, be one kind turn waste into wealth, carbon fixation and emission reduction With the method for biomass as resources.It is having recycling waste to prepare porous carbon materials as raw material using leaf waste One of efficacious prescriptions method.Moreover, the physical characteristic of its bigger serface of biomass carbon material use, can get preferable electric double layer capacitance Performance.
In the prior art, biomass carbon is increasingly becoming hot spot, Chinese patent as the electrode material of ultracapacitor CN106683899A discloses a kind of method preparing electrode material for super capacitor with wide yulan leaf, it is with wide yulan tree Leaf is raw material, is obtained through washing, drying, acidleach, charing, pickling, drying and processing.Activated carbon specific surface area obtained is up to 2534m2g-1, in 0.5A g-Discharge current under its specific capacity up to 110 F g-1.Although this method realizes wide yulan leaf Collection utilization avoids the pollution that burning disposal is brought, and realizes efficiently using for resource, but prepared porous carbon material Specific capacitance is relatively low.Consider that there is ginkgo leaf unique multilayered structure can be prepared using hydro-thermal process and KOH activating process Carbon nanosheet with the interconnection for enriching micro-/mesoporous, specific capacitance are greatly improved.
The ginkgo ornamental plant one of most popular as China, is planted in extensively on street, park and mountain, annual to produce The ginkgo leaf of thousands of tons of, the sole purpose of ginkgo leaf is extraction Cucumber as drug at present, and largely ginkgo leaf quilt Very it is waste as natural waste processing.Numerous studies both domestic and external show that the chemical composition of ginkgo leaf is sufficiently complex, main The bioactive ingredients wanted are flavonoids, terpene lactones, polypentenol and polysaccharide compound.Additionally contain organic acid, alkyl phenol Acids, amino acid, steroid, trace element etc..
These ingredients that ginkgo leaf itself has can provide nitrogen source, but specific capacitance is not too high, by adding urea Being introduced back into suitable nitrogen source makes N doping porous charcoal show excellent chemical property in EDLCs.
Therefore, it selects ginkgo leaf to expect as source, prepares biomass-based porous carbon materials, be ideal electrode of super capacitor Material.
Invention content
It is an object of the invention to provide a kind of nitrogen-doped porous carbon materials and its preparation method and application, by introducing nitrogen source, The effective surface wettability for improving carbon material, increases its fake capacitance, and using potassium hydroxide as activator, improve carbon The specific surface area of material.In addition waste's reclamation rate is improved, increases the economic value added of ginkgo leaf, reduce electrode material Production cost.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is:
N doping porous active Carbon Materials, carbon matrix precursor, nitrogenous compound and the alkali inorganic substance prepared by ginkgo leaf are directly mixed Calcination is combined to be prepared.By introducing the nitrogen sources such as urea, the surface wettability of carbon material is effectively improved, is increased Its fake capacitance, and using potassium hydroxide as activator, the specific surface area of carbon material is improved, enhance the property of ultracapacitor Energy.
Realizing the specific technical solution of the object of the invention is:
Nitrogen-doped porous carbon material is forged by ginkgo leaf after low-temperature carbonization is handled with nitrogenous compound and using alkali inorganic substance It burns activation to be prepared, specific surface area range is in 888 ~ 1132m2g-1, pore-size distribution is within the scope of 1.20 ~ 2.13nm.
The preparation method of nitrogen-doped porous carbon material includes the following steps:
Step 1)Ginkgo leaf is cleaned, is cut into fragment, drying, is placed in tube furnace at a temperature of at 400 ~ 500 DEG C, cryogenic carbon Change 1 ~ 3 h, carbonized product is filtered, washed, is dried, grinds and obtains nitrogen-doped carbon material;
Step 2)It is 1.0 in mass ratio by carbon matrix precursor and alkali inorganic substance and nitrogen source:1.0:(1.5~6.0)Mixing, is immersed in In deionized water, magnetic agitation 2 hours is put into tube furnace after drying and is calcined under nitrogen protection, and calcination activation temperature is 600 ~ 800 DEG C, 3 DEG C of heating rate, calcination soak time is 1 ~ 6 h, obtains the porous active Carbon Materials of N doping, the alkalinity nothing Machine object is any one in potassium hydroxide, sodium hydroxide, potassium carbonate, zinc chloride.
Step 3)Above-mentioned product is impregnated with hydrochloric acid solution, by washing, filtering, drying, that grinding obtains N doping is porous Carbon material.
Application of the nitrogen-doped porous carbon material as electrode material for super capacitor, when current density is 1A g-1When, than electricity Capacitance range is in 254 ~ 356 F g-1
The scanned testing electronic microscope of the present invention, the results showed that, which shows cellular porous structure.
The present invention is tested through adsorption isothermal curve and pore-size distribution, the results showed that, it is reachable with higher specific surface area 1132 m2 g-1, with a large amount of micropore and suitable mesoporous.
The present invention is through constant current charge-discharge test result, the results showed that, when current density is 1A g-1When, specific capacitance value reaches 254~356 F g-1
The present invention is through cyclic voltammetry, the results showed that, under different sweep speeds, cyclic voltammetry curve keeps good Be similar to rectangular shape, show the performance for having good electric double layer capacitance.
In order to compare the influence for whether adding nitrogen source to carbon material structure and performance, further synthesis is adulterated without additional nitrogen source Nitrogen-doped porous carbon material.Through adsorption isothermal curve and pore-size distribution test and constant current charge-discharge test, the results showed that, nothing It is 888 m that the N doping porous structure carbon material of additional nitrogen source doping, which has low specific surface area smaller,2 g-1, work as current density For 1A g-1When, specific capacitance value is 254 F g-1
Contrast test the result shows that, add obtained nitrogen-doped porous carbon material specific surface area after nitrogen source increase, aperture point Cloth is uniform, further enhances its performance of the supercapacitor.
The N doping porous structure carbon material of the present invention has the following advantages the prior art:
One, preparation process of the present invention is simple, and raw material sources are abundant, and activation temperature is not high, is easy to industrialization;
Two, it is carbon source that the present invention, which selects discarded ginkgo leaf, improves ginkgo leaf comprehensive resource utilization rate, obtains high additive value Product;
Three, nitrogen source is introduced in the present invention, more electric double layer capacitances and fake capacitance is provided for ultracapacitor;
Four, as the application of electrode material for super capacitor, when current density is 1A g-1When, specific capacitance value range 254 ~ 356 F g-1, and there is good chemical property.
Therefore, the present invention has broad application prospects in fields such as ultracapacitor, lithium ion batteries.
Description of the drawings:
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 capacitance cyclic voltammogram of nitrogen-doped porous carbon material;
Fig. 6 is the low temperature nitrogen adsorption isothermal curve of the nitrogen-doped porous carbon material adulterated without additional nitrogen source;
Fig. 7 is the pore size distribution curve of the nitrogen-doped porous carbon material adulterated without additional nitrogen source.
Specific implementation mode
The present invention is described in further detail the content of present invention by embodiment, in conjunction with Figure of description, but is not pair The limitation of the present invention.
Embodiment
Step 1)Ginkgo leaf is cleaned, is cut into fragment, drying, is placed in tube furnace at a temperature of at 500 DEG C, cryogenic carbon Change 2 h, carbonized product is filtered, washed, is dried, grinds and obtains nitrogen-doped carbon material;
Step 2)It is 1.0 in mass ratio by carbon matrix precursor and KOH and urea:3.0:1.0 mixing, are immersed in 30ml ionized waters In, magnetic agitation 2 hours is put into tube furnace after drying and is calcined under nitrogen protection, and calcination activation temperature is 700 DEG C, heating 3 DEG C of rate, calcination soak time are 2 h, obtain the porous active Carbon Materials of N doping;
Step 3)Above-mentioned product 1M HCl solutions are impregnated, and is washed with deionized, filters to neutrality, are ground after drying, Obtain nitrogen-doped porous carbon material.
By the scanned testing electronic microscope of the nitrogen-doped porous carbon material prepared in embodiment, the results are shown in Figure 1, should 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 it reaches 1132 m with higher specific surface area2 g- 1,Pore-size distribution is uniform.
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 1A g-1When, specific capacitance value is up to 356 F g-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.
In order to compare influence of the addition nitrogen source urea to carbon material structure and performance, further synthesis is adulterated without additional nitrogen source Nitrogen-doped porous carbon material, the specific steps of preparation method if not otherwise specified the step of and nitrogen-doped porous carbon material Preparation method is identical.
The difference is that:Step(2)In do not add urea.
By the nitrogen-doped porous carbon material adulterated without additional nitrogen source prepared in embodiment through adsorption isothermal curve and aperture Distribution tests, as shown in Figures 6 and 7, the N doping porous structure carbon of no additional nitrogen source doping
In summary it analyzes, the nitrogen-doped porous carbon material specific surface area and Kong Rongjun that are obtained after the addition of urea increase, aperture It is distributed uniform, further enhances its performance of the supercapacitor, specific capacity increases.

Claims (6)

1. a kind of nitrogen-doped porous carbon material, it is characterised in that:By ginkgo leaf after low-temperature carbonization is handled with nitrogenous compound and The activation of alkali inorganic substance mixed calcining is prepared, and gained nitrogen-doped porous carbon material specific surface area range is in 888 ~ 1132 m2g-1, pore-size distribution is uniform, and distribution is 1.20 ~ 2.13nm.
2. the preparation method of nitrogen-doped porous carbon material according to claim 1, which is characterized in that the method includes following Step
Step 1)Ginkgo leaf is cleaned, is cut into fragment, drying, low-temperature carbonization under certain condition is placed in tube furnace, obtains carbon Presoma;
Step 2)By step 1)Gained carbon matrix precursor is mixed with nitrogenous compound and alkali inorganic substance by certain mass ratio, go from In sub- water impregnate after, put into after drying in tube furnace nitrogen atmosphere protection under, N doping is obtained with certain condition calcining and activating Porous carbon materials;
Step 3)Above-mentioned product is impregnated with hydrochloric acid solution, it is more to obtain final N doping by washing, filtering, drying, grinding Hole carbon material.
3. preparation method according to claim 2, it is characterised in that:The step 1)Ginkgo leaf low-temperature carbonization temperature Degree is 400 ~ 500 DEG C, and carbonization time is 1 ~ 3h.
4. preparation method according to claim 2, it is characterised in that:The step 2)Nitrogenous compound be semicarbazides, Urea or guanidine carbonate, the step 2)Alkali inorganic substance be potassium hydroxide, sodium hydroxide, potassium carbonate or zinc chloride, the step Rapid 2)Nitrogen-doped carbon material and nitrogenous compound and the mass ratio of alkali inorganic substance be 1.0:1.0:(1.5~6.0).
5. preparation method according to claim 3, it is characterised in that:The step 2)Calcining and activating condition be activation Temperature is 600 ~ 800 DEG C, and soak time is 1 ~ 6 h.
6. application of the nitrogen-doped porous carbon material as electrode material for super capacitor, feature exist according to claim 1 In:When current density is 1 A g-1When, specific capacitance value range is in 254 ~ 356F g-1
CN201810456306.6A 2018-05-14 2018-05-14 A kind of preparation and its application of nitrogen-doped porous carbon material Pending CN108529621A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN108101027A (en) * 2017-12-29 2018-06-01 重庆墨希科技有限公司 Large area CVD graphenes adulterate transfer method
CN109231201A (en) * 2018-11-05 2019-01-18 安徽工业大学 A kind of preparation method of supercapacitor sulphur, nitrogen, phosphor codoping porous carbon materials
CN109319783A (en) * 2018-10-31 2019-02-12 天津科技大学 The preparation method and poplar wood base porous carbon materials product of poplar wood base porous carbon materials
CN109384212A (en) * 2018-11-17 2019-02-26 扬州工业职业技术学院 A kind of porous carbon and its application in preparation metal-supported catalyst
CN111180220A (en) * 2020-01-18 2020-05-19 温州大学 Preparation method of supercapacitor electrode material based on citrus peel biomass charcoal
CN111995964A (en) * 2020-09-04 2020-11-27 中冶赛迪技术研究中心有限公司 Novel composite nano conductive filler and preparation and application thereof

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CN106865540A (en) * 2017-03-24 2017-06-20 桂林电子科技大学 A kind of N doping loose structure carbon material and its preparation method and application
CN107128918A (en) * 2017-05-26 2017-09-05 桂林电子科技大学 A kind of preparation and its application of N doping porous active Carbon Materials

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CN106608620A (en) * 2015-10-20 2017-05-03 北京林业大学 Process for preparing nitrogen-rich active carbon from waste bamboo material
CN105565313A (en) * 2015-12-25 2016-05-11 泰山医学院附属医院 Method for rapid preparation of medical activated carbon from ginkgo leaf
CN106629651A (en) * 2016-12-20 2017-05-10 桂林电子科技大学 Nitrogen-doped carbon material with porous structure as well as preparation method and application of nitrogen-doped carbon material
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108101027A (en) * 2017-12-29 2018-06-01 重庆墨希科技有限公司 Large area CVD graphenes adulterate transfer method
CN108101027B (en) * 2017-12-29 2020-01-31 重庆墨希科技有限公司 Large-area CVD graphene doping transfer method
CN109319783A (en) * 2018-10-31 2019-02-12 天津科技大学 The preparation method and poplar wood base porous carbon materials product of poplar wood base porous carbon materials
CN109231201A (en) * 2018-11-05 2019-01-18 安徽工业大学 A kind of preparation method of supercapacitor sulphur, nitrogen, phosphor codoping porous carbon materials
CN109384212A (en) * 2018-11-17 2019-02-26 扬州工业职业技术学院 A kind of porous carbon and its application in preparation metal-supported catalyst
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CN111180220A (en) * 2020-01-18 2020-05-19 温州大学 Preparation method of supercapacitor electrode material based on citrus peel biomass charcoal
CN111995964A (en) * 2020-09-04 2020-11-27 中冶赛迪技术研究中心有限公司 Novel composite nano conductive filler and preparation and application thereof

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