CN107265436A - The preparation method and applications of biomass graphitized stephanoporate material with carbon element - Google Patents
The preparation method and applications of biomass graphitized stephanoporate material with carbon element Download PDFInfo
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- CN107265436A CN107265436A CN201710643800.9A CN201710643800A CN107265436A CN 107265436 A CN107265436 A CN 107265436A CN 201710643800 A CN201710643800 A CN 201710643800A CN 107265436 A CN107265436 A CN 107265436A
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2006/40—Electric properties
Abstract
The invention provides a kind of preparation method and applications of biomass graphitized stephanoporate material with carbon element, the preparation and living resources for belonging to carbon material utilize technical field.This method is sufficiently mixed with pore creating material/catalysts and solvents after carbonization treatment using plant as carbon source, obtains mixture；After said mixture is dried, then in inert gas atmosphere high-temperature heat treatment is carried out, finally give graphitized stephanoporate material with carbon element.The technical scheme that the present invention is provided is used as carbon source using reproducible biomass, on the basis of its intrinsic microstructure is retained, by " one-step method " while completing the porous and graphitization of carbon material, with low cost, nontoxic, environmental protection and safe and efficient can realize large-scale production；The biomass graphitized stephanoporate material with carbon element that the present invention is provided has big specific surface area and higher degree of graphitization, is suitable as electrode material and is applied to energy storage field.
Description
Technical field
Technical field is utilized the invention belongs to porous carbon materials and living resources, and in particular to a kind of biomass graphitization is more
The preparation method of hole carbon material and its application in energy field.
Background technology
The consumption requirements amount of development and the increasing fast of population with human society, traditional resource and the energy is increasingly
Greatly, environmental problem is also increasingly serious.It is to solve following energy to clean the exploitation of renewable new energy and the application of novel energy-storing technology
The feasible program of source problem, seeking suitable energy storage device and efficient energy-storage system turns into a vital research side
To.Wherein, lithium ion battery and ultracapacitor are of great interest as new energy storage device.Lithium ion battery has
Have the advantages that energy density is high, operating voltage is high, self discharge effect is small, have extended cycle life, charge efficiency is high, environmentally friendly,
It is a kind of preferable green power supply.And compared to energy storage devices such as traditional capacitors and secondary cell, ultracapacitor then has
Have that the charging interval is short, power density is high, service life length, good temp characteristic and the features such as safety and environmental protection.Therefore, lithium ion battery
It is respectively provided with and is weighed in terms of mobile communication, electronic information, electric automobile, Aero-Space and science and techniques of defence with ultracapacitor very much
Will be with wide application prospect.
Electrode material is used as the important component of the energy storage devices such as lithium ion battery and ultracapacitor, its structure, group
Into directly determining their classification and overall performance with property.In common electrode material, carbon material is because of its higher ratio
The features such as surface area, good electric conductivity, high chemical stability and cheap, abundance, is widely used as lithium ion
The electrode material of battery and ultracapacitor.In general, the principal element of influence carbon-based electrode material chemical property has：Than
Surface area, aperture, electric conductivity and surface nature etc.；Therefore, exploitation high-specific surface area, high mesoporosity, high conductivity, high-purity and
The new carbon-based electrode material of high performance-price ratio is the Research Emphasis of current high-performance energy storage device.
It is well known that reproducible natural biomass resource is because its abundant carbon content is following development of carbon material and should
With there is provided sufficient raw material sources.Often have inside the inevitable outcome competed as metabolism and natural biological, biomass
There is the multi-channel structure that nature optimizes for the absorption and transmission of ion and moisture.In general, prepared by raw material of biomass
The method of porous carbon materials is main based on chemical activation method, i.e., made with potassium hydroxide, the carbonate of potassium, sulfuric acid or zinc chloride etc.
For activator, activation pore-creating is carried out to raw material.It is real but the porous carbon that this method is obtained is based on non crystalline structure, poorly conductive
Also need to carry out high temperature graphitization processing to it when border is applied, to improve its conductivity.At present, graphited catalyst master is carried out
Will be based on molysite, such as ferric trichloride, the potassium ferricyanide.But above-mentioned activator and catalyst are generally to have severe corrosive or poison
The material of property, can cause the corrosion of production equipment and the destruction of environment.
Therefore, prepare biomass graphitized stephanoporate material with carbon element and also face following three points challenge：（1）Selection has suitable logical
The natural biomass materials of road structure；（2）Simplify operating procedure, shorten the production cycle；（3）Using the efficient pore creating material of low toxicity/
Catalyst, is reduced to equipment corrosion and environmental pollution.
The content of the invention
The problem of it is an object of the invention to exist for prior art, propose that one kind uses potassium ferrate（K2FeO4）Make
For pore creating material/catalyst, develop a kind of " one-step method " preparation method, i.e. " one-step method " and meanwhile complete the porous of carbon material with
Graphitization, realizes the green of biomass graphitized stephanoporate material with carbon element, fast and efficiently preparation method.This method have it is time-consuming less,
Simple to operate, nontoxic, environmentally friendly the features such as, product has big specific surface area, high degree of graphitization and electric conductivity,
Suitable for large-scale industrialization production, and the practical application in energy storage field.
The technical solution adopted by the present invention is specific as follows：
A kind of preparation method and applications of biomass graphitized stephanoporate material with carbon element, it is characterised in that this method includes following step
Suddenly：
（1）Fresh biological material is cleaned, dried, tube furnace is then transferred under inert gas shielding in 200 ~ 800 DEG C
In the range of carry out carbonization 1 ~ 4 hour, obtain biomass carbonization material；
（2）Biomass carbonization material according to a certain ratio, pore creating material/catalysts and solvents are uniformly mixed, are then dried；
Pore creating material/the catalyst is potassium ferrate, and the material is simultaneously as the pore creating material and graphited catalyst of material；It is described molten
Agent is water；
（3）Said mixture is transferred in tube furnace and is heat-treated, in 600 ~ 1500 DEG C of scopes under inert gas shielding
Inside holding 1 ~ 6 hour；Reaction product is by multiple Diluted Acid Washing, washing and dries, and finally gives biomass graphitization porous carbon
Material.
Step（1）Described in biological material be bamboo, wheat, paddy rice, corn, rape, cotton, the stalk of sugarcane in
At least one is used as carbon source.
Step（2）Described in the mass ratio of biomass carbonization material and pore creating material/catalyst be 1:10~5:1.
Step（3）Middle heat treatment temperature is 800 ~ 100 DEG C；Soaking time is 2 ~ 4 hours.
Step（1）With（3）Described in inert gas be at least one of argon gas, helium and nitrogen.
In above-mentioned preparation method, only with potassium ferrate simultaneously as pore creating material and catalyst, and other any work are added without
Agent or catalyst.
A kind of biomass graphitized stephanoporate material with carbon element, is prepared by above-mentioned preparation method.
Above-mentioned biomass graphitized stephanoporate material with carbon element as electrode material energy storage field application.
The invention provides the biomass graphitized stephanoporate material with carbon element that above-mentioned technical proposal methods described is prepared, it compares
Surface area is 1000 ~ 2000 m2/ g, and with higher degree of graphitization, sharp correspondence is observed in X ray diffracting spectrum
In graphite-structure（002）The intensity rate at D peaks and G peaks is less than 0.7 in the diffraction maximum of crystal face, Raman spectrum.The invention provides
The biomass graphitized stephanoporate material with carbon element that above-mentioned technical proposal methods described is prepared is as energy storage device electrode material in energy
The application of source domain.For example, it can provide 222.3 F/ as electrode material for super capacitor under 0.5 A/g current density
G capacitance, and with excellent high rate performance.
The present invention compared with prior art, with advantages below and beneficial effect：
（1）The present invention using bamboo and agricultural crop straw as carbon source, these inside plants have naturally occur be available for ion,
The multi-channel structure that hydrone is quickly transmitted, constructs the basic framework as high performance electrode material；And all raw materials are
Renewable resource or agriculture and forestry organic waste material, abundance are with low cost, environmental protection.
（2）Compared with prior art, the present invention uses " one-step method " while completing the porous and graphitization of carbon material, profit
Use potassium ferrate（K2FeO4）Simultaneously as pore creating material/catalyst, operating procedure is simplified, the production cycle is shortened.
（3）The potassium ferrate being related in the present invention（K2FeO4）, sewage disposal is commonly used for, is a kind of new green ring
Protect material.It is not related to the participation and generation of any polluter in the preparation process of the biomass graphitized stephanoporate material with carbon element, is
A kind of nontoxic, environmental protection, preparation method rapidly and efficiently, a kind of new method is provided for the industrialized production of porous carbon materials
And new approaches, with important application value and wide market potential.
Brief description of the drawings
Fig. 1 is the SEM of the biomass graphitized stephanoporate material with carbon element prepared in the embodiment of the present invention 1（SEM）
Figure.
Fig. 2 is the specific surface area of the biomass graphitized stephanoporate material with carbon element prepared in the embodiment of the present invention 1（BET）As a result
Figure.
Fig. 3 is the X-ray diffraction of the biomass graphitized stephanoporate material with carbon element prepared in the embodiment of the present invention 1（XRD）Figure.
Fig. 4 is the Raman spectrum of the biomass graphitized stephanoporate material with carbon element prepared in the embodiment of the present invention 1（Raman）Figure.
Fig. 5 be in the embodiment of the present invention 2 the biomass graphitized stephanoporate material with carbon element for preparing as electrode of super capacitor material
Material, the cyclic voltammetry curve under different scanning speed.
Fig. 6 be in the embodiment of the present invention 2 the biomass graphitized stephanoporate material with carbon element for preparing as electrode of super capacitor material
Material, the charging and discharging curve under different current densities.
Fig. 7 be in the embodiment of the present invention 2 the biomass graphitized stephanoporate material with carbon element for preparing as electrode of super capacitor material
Material, the specific capacity under different current densities.
Fig. 8 be in the embodiment of the present invention 3 the biomass graphitized stephanoporate material with carbon element for preparing as electrode of super capacitor material
Material, the specific capacity under different current densities.
Fig. 9 be in the embodiment of the present invention 4 the biomass graphitized stephanoporate material with carbon element for preparing as electrode of super capacitor material
Material, the specific capacity under different current densities.
Embodiment
The present invention is further elaborated with reference to the accompanying drawings and examples, but therefore not limited the present invention to described
Scope of embodiments within.
Embodiment 1
The bamboo pole that part is fresh is taken, is shredded, cleaned, dried, is then transferred in tube furnace and enters under argon gas protection in 400 DEG C
Row carbonization 2 hours, obtains the char-forming material of bamboo；By 0.60g char-forming material, 0.99g potassium ferrates（K2FeO4）With 45ml water
Uniform mixing, is then dried；Said mixture is transferred in tube furnace and is heat-treated, in 800 under argon gas protection
DEG C insulation 2 hours；Reaction product is passed through multiple watery hydrochloric acid and washing, dried, and finally gives biomass graphitized stephanoporate material with carbon element.
Electron microscope is scanned to above-mentioned biomass graphitized stephanoporate material with carbon element（SEM）Observation, its pattern such as Fig. 1 institutes
Show.As seen from Figure 1, the biomass graphitized stephanoporate material with carbon element of preparation has obvious three-dimensional porous structure.To the life
Material graphitized stephanoporate material with carbon element carries out specific surface area test, obtains the N of the material2Adsorption desorption curve map, as shown in Figure 2.Survey
Examination structure shows that the biomass graphitized stephanoporate material with carbon element has 1638.13m2/ g specific surface area.According to Fig. 3 and Fig. 4, XRD
Correspondence graphite in spectral line（002）With（101）The appearance of diffraction maximum, it was demonstrated that material has certain graphite-structure；In Raman spectrum
The ratio at relatively low D/G peaks（ID/IG=0.62）And the appearance at 2D peaks illustrates that the biomass graphitized stephanoporate material with carbon element is higher
Degree of graphitization, i.e., successfully prepared graphitized stephanoporate material with carbon element.
Embodiment 2
The bamboo pole that part is fresh is taken, is shredded, cleaned, dried, is then transferred in tube furnace and enters under argon gas protection in 500 DEG C
Row carbonization 1 hour, obtains the char-forming material of bamboo；By 0.60g char-forming material, 0.99g potassium ferrates（K2FeO4）With 45ml water
Uniform mixing, is then dried；Said mixture is transferred in tube furnace and is heat-treated, in 1000 under argon gas protection
DEG C insulation 1 hour；Reaction product is passed through multiple watery hydrochloric acid and washing, dried, and finally gives biomass graphitized stephanoporate material with carbon element.
It is 8 to weigh mass ratio:1:The 1 biomass graphitized stephanoporate material with carbon element, acetylene black and polyvinylidene fluoride
（PVDF）, it is transferred into mortar, adds a small amount of 1-METHYLPYRROLIDONE（N-Methyl pyrrolidone, NMP）As
Solvent, is fully ground to pasty state, mixture is coated in the foam nickel sheet that size is the mm of 2 mm * 1, then at 120 DEG C
Vacuum drying 12 hours, finally in 10Mpa pressure lower sheeting 1 minute, obtains electrode of super capacitor.
The carbon electrode for choosing the biomass graphitized stephanoporate material with carbon element preparation obtained by the present embodiment is working electrode, 1 mm
* 1 mm platinized platinums are that, to electrode, Ag/AgCl is reference electrode, 6mol KOH solutions are electrolyte, are carried out with electrochemical workstation
Cyclic voltammetry and constant current charge-discharge test, voltage window are -1.0 ~ 0V, and voltage sweeps speed and takes 5,10,20,50,80 respectively,
100mV/s, current density takes 1,2,5,8,10A/g respectively.As shown in figure 5, the cyclic voltammetry curve of the electrode is smooth, symmetry
Well, in the case that height sweeps speed, more complete rectangle can be also showed, the excellent capacitance characteristic of electrode is reflected.
As shown in fig. 6, CP curves show symmetrical isosceles triangle shape, illustrate that it has typical electric double layer capacitance characteristic.Such as Fig. 7
Shown, the electrode can provide 222.3 F/g capacitance under 0.5 A/g current density, and when current density increases to 20
Still there is 115.0 F/g capacitance during A/g.Above test result shows the porous carbon-based electrode of biomass graphitization as super
Electrode for capacitors has considerable energy-storage property and excellent high rate performance.
Embodiment 3
Discarded maize straw is taken, is shredded, cleaned, dried, be then transferred in tube furnace and enter under nitrogen protection in 400 DEG C
Row carbonization 4 hours, obtains the char-forming material of maize straw；By 0.60g char-forming material, 6.0g potassium ferrates（K2FeO4）With
50ml water is uniformly mixed, and is then dried；Said mixture is transferred in tube furnace and is heat-treated, under argon gas protection
6 hours are incubated in 1500 DEG C；Reaction product is passed through multiple watery hydrochloric acid and washing, dried, and finally gives biomass graphitization porous
Carbon material.The carbon electrode for choosing the biomass graphitized stephanoporate material with carbon element preparation obtained by the present embodiment is working electrode, is carried out
Constant current charge-discharge test simultaneously calculates the capacitance under different current densities.The electrode has under 0.5A/g current density
163.2 F/g capacitance.
Embodiment 4
Discarded cotton stalk is taken, is shredded, cleaned, dried, be then transferred in tube furnace and enter under nitrogen protection in 400 DEG C
Row carbonization 4 hours, obtains the char-forming material of cotton stalk；By 0.60g char-forming material, 0.12g potassium ferrates（K2FeO4）With
50ml water is uniformly mixed, and is then dried；Said mixture is transferred in tube furnace and is heat-treated, under argon gas protection
6 hours are incubated in 600 DEG C；Reaction product is passed through multiple watery hydrochloric acid and washing, dried, and finally gives biomass graphitization porous carbon
Material.The carbon electrode for choosing the biomass graphitized stephanoporate material with carbon element preparation obtained by the present embodiment is working electrode, is carried out permanent
Stream charge-discharge test simultaneously calculates the capacitance under different current densities.The electrode has 149.8 under 0.5A/g current density
F/g capacitance.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of biomass graphitized stephanoporate material with carbon element, it is characterised in that comprise the following steps：
(1) fresh biological material is cleaned, dried, be then transferred to tube furnace under inert gas shielding in 200~800 DEG C
In the range of carry out carbonization 1~4 hour, obtain biomass carbonization material；
(2) biomass carbonization material according to a certain ratio, pore creating material/catalysts and solvents are uniformly mixed, are then dried；
Pore creating material/the catalyst is potassium ferrate, and the material is simultaneously as the pore creating material and graphited catalyst of material；It is described molten
Agent is water；
(3) said mixture is transferred in tube furnace and be heat-treated, in 600~1500 DEG C of scopes under inert gas shielding
Inside holding 1~6 hour；Reaction product is by multiple Diluted Acid Washing, washing and dries, and finally gives biomass graphitization porous carbon
Material.
2. preparation method according to claim 1, it is characterised in that：Biological material described in step (1) is bamboo, small
At least one of wheat, paddy rice, corn, rape, cotton, stalk of sugarcane are used as carbon source.
3. preparation method according to claim 1, it is characterised in that：Biomass carbonization material is with making described in step (2)
The mass ratio of hole agent/catalyst is 1:10~5:1.
4. preparation method according to claim 1, it is characterised in that：Heat treatment temperature is 800~100 DEG C in step (3)；
Soaking time is 2~4 hours.
5. preparation method according to claim 1, it is characterised in that：Inert gas described in step (1) and (3) is argon
At least one of gas, helium and nitrogen.
6. preparation method according to claim 1, it is characterised in that：In above-mentioned preparation method, only with potassium ferrate simultaneously
As pore creating material and catalyst, and it is added without other any activators or catalyst.
7. a kind of biomass graphitized stephanoporate material with carbon element, it is characterised in that：As the preparation side any one of claim 1-6
Method is prepared.
8. biomass graphitized stephanoporate material with carbon element according to claim 7 as electrode material energy storage field application.
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| CN108109853A (en) * | 2017-12-25 | 2018-06-01 | 武汉大学 | The preparation method and application of superelevation specific surface porous carbon biomass electrode material |
| CN108439401A (en) * | 2018-04-19 | 2018-08-24 | 句容市盛达环保净化材料有限公司 | A kind of preparation method of activated carbon |
| CN108557799A (en) * | 2018-06-04 | 2018-09-21 | 河南工程学院 | A kind of high-purity high conductivity class graphene grading-hole porous charcoal and preparation method thereof |
| CN108557816A (en) * | 2018-06-26 | 2018-09-21 | 武汉大学 | A kind of preparation method of high specific surface area porous graphitized charcoal |
| CN108726576A (en) * | 2018-06-01 | 2018-11-02 | 东莞理工学院 | Carbonization-activation oxidation is continuous to prepare porous charcoal/Fe3O4Method |
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| CN108439401A (en) * | 2018-04-19 | 2018-08-24 | 句容市盛达环保净化材料有限公司 | A kind of preparation method of activated carbon |
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| CN113842938A (en) * | 2021-09-18 | 2021-12-28 | 河北零点新能源科技有限公司 | Novel g-C3N4Method for preparing derived carbonaceous adsorbent and photocatalytic material |
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