CN105914372A - Three-dimensional porous biomass carbon nanomaterial prepared from pomace, and preparation method and application therefor - Google Patents
Three-dimensional porous biomass carbon nanomaterial prepared from pomace, and preparation method and application therefor Download PDFInfo
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- CN105914372A CN105914372A CN201610473908.3A CN201610473908A CN105914372A CN 105914372 A CN105914372 A CN 105914372A CN 201610473908 A CN201610473908 A CN 201610473908A CN 105914372 A CN105914372 A CN 105914372A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a three-dimensional porous biomass carbon nanomaterial prepared from pomace, and a preparation method and an application therefor, and belongs to the preparation technical field of an electrode material of a sodium ion battery. An activated pomace precursor is prepared firstly by a hydrothermal method; and then the precursor is condensed and directly passes through a tubular atmosphere furnace to obtain the biomass active carbon material with the three-dimensional porous nanostructure. The three-dimensional porous biomass carbon nanomaterial is simple in preparation method, high in uniformity, easy to control the process, high in product repeatability and capable of promoting the large-scale production; and the three-dimensional porous biomass carbon nanomaterial prepared by the method has excellent conductivity and cycling stability and high specific discharge capacity, so that the three-dimensional porous biomass carbon nanomaterial can be widely used as the negative electrode material of the sodium ion battery.
Description
Technical field
The invention belongs to sodium ion battery electrode material preparing technical field, be specifically related to one and utilize marc system
Standby three-dimensional porous biomass carbon nano material and preparation method and application.
Background technology
At present, lithium ion battery is occupied an leading position in we live, but is as battery industry, intelligent grid
Development, limited lithium resource will be unable to the demand meeting people to it.Due to sodium aboundresources, and open
Send out low cost, and sodium and lithium are same major elements, so it is well can one of the resource that substitute lithium ion.
Generally lithium battery is using graphite as negative pole, but when graphite is for sodium-ion battery, due to sodium ion
Radius is relatively big, well can not carry out reversible deintercalation in graphite linings, so its electrochemistry of showing
Performance is not fine, capacity about 25mAh g-1.Sodium-ion battery is studied more carbon negative pole material
For hard carbon, the capacity of general hard carbon class material about can reach 100mAh g-1。[Lotfabad,E.M.,Ding,
J.,Cui,K.,Kohandehghan,A.,Kalisvaart,W.P.,Hazelton,M.,&Mitlin,D.(2014).
High-density sodium and lithium ion battery anodes from banana peels.Acs Nano,
8(7),7115-7129.]
Along with raising and the increase of fruit juice factory of people's quality of life, more and more discard marc, due to
Processing mode is improper, result in substantial amounts of bacterial reproduction, damages environment.At about 2000,
Marc the most once caused the most serious pollution, in recent years, in order to reduce marc to rivers, soil, air
Produced harm, the secondary of marc utilizes increasingly to be paid attention to by people.But it is presently mainly it is entered
The processing mode that row is extensive, as animal feed or fertilizer are processed in dry in the sun, pulverizing etc., utilizes marc to make
Wine, makes fruit jam etc..[Li Juxiu, Li Zhixi, Yang Mingquan, Jia Aijuan. (2002). combining of apple pomace resource
Close and utilize. " Journal of Northwest Sci Tech University of Agriculture and Forestry ", natural science edition, (z1), 103-106.].
Summary of the invention
It is an object of the invention to provide a kind of three-dimensional porous biomass carbon nano material utilizing marc to prepare
And preparation method and application, the method have simple to operate, productivity is high, energy consumption is low, the feature such as reproducible,
Anode material of lithium-ion battery prepared by the three-dimensional porous biomass carbon nano material prepared by the method has
The features such as specific discharge capacity is high, good cycling stability.
The present invention is to be achieved through the following technical solutions:
The invention discloses a kind of method utilizing marc to prepare three-dimensional porous biomass carbon nano material, including
Following steps:
1) press Fructus Mali pumilae marc and KOH=1:(0.3～1.5) mass ratio, take Fructus Mali pumilae marc and KOH, fill
After dividing mixing, carry out hydro-thermal reaction；
2) after hydro-thermal reaction terminates, it is cooled to room temperature, products therefrom heating is concentrated, prepares presoma；
3) under an argon atmosphere, by presoma with the programming rate of 5～15 DEG C/min, it is warming up to from room temperature
60～100 DEG C, it is incubated 0.3～0.7h, is then warming up to 500～900 DEG C with 5～15 DEG C/min, and is incubated
1.5～3.5h；
4) by step 3) prepare product cleaning, be dried, prepare three-dimensional porous biomass carbon nano material.
Step 1) described hydro-thermal reaction, be Fructus Mali pumilae marc and KOH are fully mixed after, be placed in reactor
In, with the programming rate of 5～15 DEG C/min, from room temperature, rise to 160～200 DEG C, be incubated 18～30h.
Step 3) in, the volume flow of argon controls 20～100sccm.
Step 4) described in cleaning be that product deionized water and dehydrated alcohol are cleaned 2～6 times successively.
Step 4) described in dry be at 50～90 DEG C, be dried 12～24h.
The invention also discloses the three-dimensional porous biomass carbon nano material using said method to prepare.
The invention also discloses above-mentioned three-dimensional porous biomass carbon nano material and prepare sodium-ion battery electrode
Application in material.
Compared with prior art, the present invention has a following useful technique effect:
The method utilizing marc to prepare three-dimensional porous biomass carbon nano material disclosed by the invention, utilizes marc
For biomass sources by, after hydro-thermal, carbonization, obtaining the carbon nanomaterial of three-dimensional porous structure.The method is passed through
Add KOH, saccharide, solable matter in removable marc during hydro-thermal when hydro-thermal, also act as activation and make
With and preliminary pore-creating effect, by concentrating, and then directly carry out tube-type atmosphere furnace carbonization, it is not necessary to add
Other pore creating material, direct condensed water hot after hydro-thermal completes, by the condition of conservative control argon, with
Given pace heats up and synthesizes three-dimensional porous nano carbon structure material.The three-dimensional porous life that the inventive method synthesizes
Material carbon nanomaterial makes a big difference with traditional structure two-dimensional structure, and it has three-D space structure, relatively
Big hole diameter, thus provide the micro-space of sufficiently large reaction to sodium ion so that it is can be easy to into
Row deintercalation, and three dimensional structure well avoid its embedding de-during the caving in of recurring structure, improve
The cyclical stability of material and electric conductivity.Preparation method of the present invention is simple, and homogeneity is good, and process is easily-controllable, produces
The repeatability of thing is high, beneficially large-scale production.
The three-dimensional porous biomass carbon nano material prepared through the inventive method shows the electric conductivity of excellence, follows
Ring stability and high specific discharge capacity, it is possible to be widely used as anode material of lithium-ion battery.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the three-dimensional porous biomass carbon nano material of preparation；
Fig. 2 is the electromicroscopic photograph of the three-dimensional porous biomass carbon nano material of preparation；Wherein, (a) is
FESEM schemes, and (b) is HRTEM figure；
Fig. 3 is that the three-dimensional porous biomass carbon nano material of preparation is tested for the cycle performance of sodium-ion battery
Figure.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, described in the present invention
Explain rather than limit.
Embodiment 1
A kind of method utilizing marc to prepare three-dimensional porous biomass carbon nano material, comprises the following steps:
1) preparation of presoma biomass carbon
1. weigh the scrubbed dried Fructus Mali pumilae marc of 3.5g to mix with 1.05g KOH, add 50ml distillation
Water, in reactor, is sufficiently mixed, stirs；
2. rise to 160 DEG C with the heating rate of 5 DEG C/min, be incubated 18h；
3. reaction is cooled to room temperature after terminating；By product evaporation and concentration, prepare biomass carbon presoma.
2) preparation of porous three-dimensional biomass carbon
1. weigh the biomass carbon presoma of 1g in porcelain boat, and porcelain boat is placed in tube-type atmosphere furnace；
2. it is passed through the argon that volume flow is 20sccm, is warming up to 60 DEG C with the programming rate of 5 DEG C/min,
Insulation 0.7h；
3. with the programming rate of 5 DEG C/min, from 60 DEG C, it is warming up to 500 DEG C, begins to cool down after insulation 3.5h
To room temperature；
4. product deionized water is cleaned 2 times, by washes of absolute alcohol 2 times, vacuum under the conditions of 50 DEG C
It is dried 12h, i.e. obtains the three-dimensional porous biomass carbon of end product.
Seeing Fig. 1, can obtain from Fig. 1, there is " steamed bread " shape peak of standard when about 25 ° in 2-theta angle,
May determine that it is amorphous state.
Seeing Fig. 2, (a) is the FESEM figure of biomass carbon, it can be seen that it is tied for three-dimensional communication
Structure, has abundant pore space structure, and aperture is about 500nm, and even size distribution, and dispersibility is preferable.
B () is HRTEM figure, there it can be seen that its aperture is about 500nm, and even size distribution,
Dispersibility is preferable, and this is Na+Embedding and abjection provide good condition.
Embodiment 2
A kind of method utilizing marc to prepare three-dimensional porous biomass carbon nano material, comprises the following steps:
1) preparation of presoma biomass carbon
1. weigh the scrubbed dried Fructus Mali pumilae marc of 4.5g to mix with 2.25g KOH, add 50mL and steam
Distilled water, in reactor, is sufficiently mixed, stirs；
2. rise to 170 DEG C with the heating rate of 7 DEG C/min, be incubated 21h；
3. reaction is cooled to room temperature after terminating；By product evaporation and concentration, prepare biomass carbon presoma.
2) preparation of porous three-dimensional biomass carbon
1. weigh the biomass carbon presoma of 2g in porcelain boat, and porcelain boat is placed in tube-type atmosphere furnace；
2. it is passed through the argon that volume flow is 40sccm, is warming up to 70 DEG C with the programming rate of 7 DEG C/min,
Insulation 0.6h, to get rid of the moisture of residual in sample；
3. with the programming rate of 7 DEG C/min, from 70 DEG C, it is warming up to 600 DEG C, begins to cool down after insulation 3.0h
To room temperature；
4. product deionized water is cleaned 3 times, by washes of absolute alcohol 3 times, vacuum under the conditions of 60 DEG C
It is dried 15h, i.e. obtains the three-dimensional porous biomass carbon of end product.
Embodiment 3
A kind of method utilizing marc to prepare three-dimensional porous biomass carbon nano material, comprises the following steps: 1)
The preparation of presoma biomass carbon
1. weigh the scrubbed dried Fructus Mali pumilae marc of 5.5g to mix with 3.85g KOH, add 50ml distillation
Water, in reactor, is sufficiently mixed, stirs；
2. rise to 180 DEG C with the heating rate of 10 DEG C/min, be incubated 24h；
3. reaction is cooled to room temperature after terminating；By product evaporation and concentration, prepare biomass carbon presoma.
2) preparation of porous three-dimensional biomass carbon
1. weigh the biomass carbon presoma of 3g in porcelain boat, and porcelain boat is placed in tube-type atmosphere furnace；
2. it is passed through the argon that volume flow is 60sccm, is warming up to 80 DEG C with the programming rate of 10 DEG C/min,
Insulation 0.5h, to get rid of the moisture of residual in sample；
3. with the programming rate of 10 DEG C/min, from 80 DEG C, it is warming up to 700 DEG C, starts cold after insulation 2.5h
But to room temperature；
4. product deionized water is cleaned 4 times, by washes of absolute alcohol 4 times, vacuum under the conditions of 70 DEG C
It is dried 18h, i.e. obtains the three-dimensional porous biomass carbon of end product.
Embodiment 4
A kind of method utilizing marc to prepare three-dimensional porous biomass carbon nano material, comprises the following steps:
1) preparation of presoma biomass carbon
1. weigh the scrubbed dried Fructus Mali pumilae marc of 6.5g to mix with 5.85g KOH, add 50ml distillation
Water, in reactor, is sufficiently mixed, stirs；
2. rise to 190 DEG C with the heating rate of 12 DEG C/min, be incubated 27h；
3. reaction is cooled to room temperature after terminating；By product evaporation and concentration, prepare biomass carbon presoma.
2) preparation of porous three-dimensional biomass carbon
1. weigh the biomass carbon presoma of 4g in porcelain boat, and porcelain boat is placed in tube-type atmosphere furnace；
2. it is passed through the argon that volume flow is 80sccm, is warming up to 90 DEG C with the programming rate of 12 DEG C/min,
Insulation 0.4h, to get rid of the moisture of residual in sample；
3. with the programming rate of 12 DEG C/min, from 90 DEG C, it is warming up to 800 DEG C, starts cold after insulation 2.0h
But to room temperature；
4. product deionized water is cleaned 5 times, by washes of absolute alcohol 5 times, vacuum under the conditions of 80 DEG C
It is dried 21h, i.e. obtains the three-dimensional porous biomass carbon of end product.
Embodiment 5
A kind of method utilizing marc to prepare three-dimensional porous biomass carbon nano material, comprises the following steps:
1) preparation of presoma biomass carbon
1. weigh the scrubbed dried Fructus Mali pumilae marc of 7.5g to mix with 11.25g KOH, add 50ml and steam
Distilled water, in reactor, is sufficiently mixed, stirs；
2. rise to 200 DEG C with the heating rate of 15 DEG C/min, be incubated 30h；
3. reaction is cooled to room temperature after terminating；By product evaporation and concentration, prepare biomass carbon presoma.
2) preparation of porous three-dimensional biomass carbon
1. weigh the biomass carbon presoma of 5g in porcelain boat, and porcelain boat is placed in tube-type atmosphere furnace；
2. it is passed through the argon that volume flow is 100sccm, is warming up to 100 DEG C with the programming rate of 15 DEG C/min
, it is incubated 0.3h, to get rid of the moisture of residual in sample；
3. with the programming rate of 15 DEG C/min, from 100 DEG C, it is warming up to 900 DEG C, starts cold after insulation 1.5h
But to room temperature；
4. product deionized water is cleaned 6 times, by washes of absolute alcohol 6 times, vacuum under the conditions of 90 DEG C
It is dried 24h, i.e. obtains the three-dimensional porous biomass carbon of end product.
Seeing Fig. 3, can obtain from Fig. 3, the active carbon material of the three-dimensional porous structure prepared is in electric current density 100
It is 335mAh/g that mA/g records its reversible capacity, and after circulation 80 circle, its capacity is still maintained at 203mAh
/ g, its coulombic efficiency is maintained at about 99.0%, shows that the activated carbon from activated sludge of this three dimensional structure has higher
Specific discharge capacity and stable cycle performance.
In sum, the inventive method mentality of designing is novel, by hydro-thermal tube-type atmosphere furnace reaction method, with
And the control to noble gas, the control to other factors, the biomass of the three dimensional structure preparing porous are lived
Property charcoal, thus give the micro-space of reaction that ion is sufficient, and improve the cyclical stability of material.Simultaneously
Additionally, preparation process of the present invention is easily-controllable, the cycle is short, and the repeatability of product is high, and productivity is big, beneficially scale
Metaplasia is produced.The biomass active carbon prepared through the method has stable three-dimensional for anode material of lithium-ion battery
Space structure, abundant pore space structure, and also its specific discharge capacity is high, good cycling stability, coulombic efficiency
High.
Claims (7)
1. one kind utilizes the method that marc prepares three-dimensional porous biomass carbon nano material, it is characterised in that
Comprise the following steps:
1) press Fructus Mali pumilae marc and KOH=1:(0.3～1.5) mass ratio, take Fructus Mali pumilae marc and KOH, fill
After dividing mixing, carry out hydro-thermal reaction；
2) after hydro-thermal reaction terminates, it is cooled to room temperature, products therefrom heating is concentrated, prepares presoma；
3) under an argon atmosphere, by presoma with the programming rate of 5～15 DEG C/min, it is warming up to from room temperature
60～100 DEG C, it is incubated 0.3～0.7h, is then warming up to 500～900 DEG C with 5～15 DEG C/min, and is incubated
1.5～3.5h；
4) by step 3) prepare product cleaning, be dried, prepare three-dimensional porous biomass carbon nano material.
The side utilizing marc to prepare three-dimensional porous biomass carbon nano material the most according to claim 1
Method, it is characterised in that step 1) described hydro-thermal reaction, be Fructus Mali pumilae marc and KOH are fully mixed after,
It is placed in reactor, with the programming rate of 5～15 DEG C/min, from room temperature, rises to 160～200 DEG C, insulation
18～30h.
The side utilizing marc to prepare three-dimensional porous biomass carbon nano material the most according to claim 1
Method, it is characterised in that step 3) in, the volume flow of argon controls 20～100sccm.
The side utilizing marc to prepare three-dimensional porous biomass carbon nano material the most according to claim 1
Method, it is characterised in that step 4) described in cleaning be by the most clear to product deionized water and dehydrated alcohol
Wash 2～6 times.
The side utilizing marc to prepare three-dimensional porous biomass carbon nano material the most according to claim 1
Method, it is characterised in that step 4) described in dry be at 50～90 DEG C, be dried 12～24h.
6. use the three-dimensional porous biomass carbon nanometer that in Claims 1 to 5, method described in any one prepares
Material.
7. the three-dimensional porous biomass carbon nano material described in claim 6 is preparing sodium-ion battery electrode
Application in material.
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Cited By (15)
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| CN106517181A (en) * | 2016-10-25 | 2017-03-22 | 武汉理工大学 | Preparation method of biomass based activated carbon with high CO2 adsorption efficiency |
| CN106532049A (en) * | 2016-12-27 | 2017-03-22 | 陕西科技大学 | Preparation method of carbon electrode material of porous structure sodium-ion battery |
| CN106784704A (en) * | 2016-12-27 | 2017-05-31 | 陕西科技大学 | A kind of preparation method of N doping charcoal carbon negative pole material |
| CN106915737A (en) * | 2016-12-07 | 2017-07-04 | 南昌大学 | A kind of preparation method of carbon nanosheet aeroge |
| CN107459037A (en) * | 2017-08-02 | 2017-12-12 | 四川大学 | A kind of method of low temperature preparation carbon material coproduction fertilizer |
| CN107871869A (en) * | 2017-09-25 | 2018-04-03 | 桂林理工大学 | Adulterate the preparation method and applications of sisal fiber Quito pore carbon electrode material |
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| CN109305678A (en) * | 2018-11-21 | 2019-02-05 | 济宁学院 | A kind of active carbon with high specific surface area electrode material and preparation method thereof |
| CN109473295A (en) * | 2017-09-07 | 2019-03-15 | 北京化工大学 | A method of electrode of super capacitor carbon material is prepared using apple |
| CN109809402A (en) * | 2019-01-14 | 2019-05-28 | 陕西科技大学 | A kind of preparation method being used for sodium-ion battery material with three-dimensional hollow porous carbon made of pomace |
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| CN107871869B (en) * | 2017-09-25 | 2019-10-11 | 桂林理工大学 | Adulterate the preparation method and applications of sisal fiber Quito pore carbon electrode material |
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| CN109305678A (en) * | 2018-11-21 | 2019-02-05 | 济宁学院 | A kind of active carbon with high specific surface area electrode material and preparation method thereof |
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