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 PDFInfo
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- 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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- Prior art keywords
- nitrogen
- carbon material
- porous carbon
- ginkgo leaf
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
-
- 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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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 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
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。
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| 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 |
| CN109987603A (en) * | 2019-03-18 | 2019-07-09 | 毛舜义 | A kind of preparation method of the biomass-based electrode material of N doping porous carbon |
| CN110526243A (en) * | 2019-07-29 | 2019-12-03 | 桂林理工大学 | A kind of preparation method and applications of the biomass porous carbon of supercapacitor |
| CN111180220A (en) * | 2020-01-18 | 2020-05-19 | 温州大学 | Preparation method of supercapacitor electrode material based on citrus peel biomass charcoal |
| CN111196601A (en) * | 2020-01-19 | 2020-05-26 | 桂林理工大学 | Super capacitor electrode material and preparation method and application thereof |
| CN111362266A (en) * | 2020-02-28 | 2020-07-03 | 华南农业大学 | High-yield nitrogen-doped porous carbon material and preparation method and application thereof |
| 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 |
| CN112250068A (en) * | 2020-09-25 | 2021-01-22 | 桂林电子科技大学 | Biomass osmanthus fragrans porous carbon material and preparation method and application thereof |
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| 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 |
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| CN111362266A (en) * | 2020-02-28 | 2020-07-03 | 华南农业大学 | High-yield nitrogen-doped porous carbon material and preparation method and application thereof |
| CN111362266B (en) * | 2020-02-28 | 2022-07-05 | 华南农业大学 | High-yield nitrogen-doped porous carbon material and preparation method and application thereof |
| 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 |
| CN112250068A (en) * | 2020-09-25 | 2021-01-22 | 桂林电子科技大学 | Biomass osmanthus fragrans porous carbon material and preparation method and application thereof |
| CN112938967A (en) * | 2021-05-07 | 2021-06-11 | 桂林电子科技大学 | Fermented bean curd-based porous carbon material and preparation method and application 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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| CN114678538A (en) * | 2022-01-07 | 2022-06-28 | 齐鲁工业大学 | Biomass-derived porous carbon as positive electrode material of zinc-iodine battery |
| CN114735698A (en) * | 2022-04-11 | 2022-07-12 | 中国计量大学 | Nitrogen and/or phosphorus adsorption doped material and preparation method and application thereof |
| CN114735698B (en) * | 2022-04-11 | 2023-12-22 | 中国计量大学 | Nitrogen and/or phosphorus adsorption doping material, and preparation method and application thereof |
| CN114988405A (en) * | 2022-05-23 | 2022-09-02 | 海南师范大学 | Preparation method and application of broadleaf holly leaf biological porous carbon material |
| CN114988405B (en) * | 2022-05-23 | 2023-12-29 | 海南师范大学 | Preparation method and application of kuding tea biological porous carbon material |
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