CN105914372B - A kind of three-dimensional porous biomass carbon nano material and preparation method and application prepared using pomace - Google Patents
A kind of three-dimensional porous biomass carbon nano material and preparation method and application prepared using pomace Download PDFInfo
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- CN105914372B CN105914372B CN201610473908.3A CN201610473908A CN105914372B CN 105914372 B CN105914372 B CN 105914372B CN 201610473908 A CN201610473908 A CN 201610473908A CN 105914372 B CN105914372 B CN 105914372B
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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 kind of three-dimensional porous biomass carbon nano materials and preparation method and application prepared using pomace, belong to sodium ion battery electrode material preparation technical field.The pomace presoma for preparing activation by hydro-thermal first, directly by tube-type atmosphere furnace, is prepared with three-dimensional porous nanostructure biomass active Carbon Materials after concentration.Preparation method of the present invention is simple, and homogeneity is good, and process is easily-controllable, and the repeatability of product is high, is conducive to large-scale production.Three-dimensional porous biomass carbon nano material is made through the method for the present invention and shows excellent electric conductivity, cyclical stability and high specific discharge capacity, can be widely used as anode material of lithium-ion battery.
Description
Technical field
The invention belongs to sodium ion battery electrode material preparation technical fields, and in particular to a kind of to utilize the three of pomace preparation
Tie up multiporous biological matter carbon nanomaterial and preparation method and application.
Background technique
Currently, lithium ion battery is occupied an leading position in we live, but with the development of battery industry, smart grid,
Limited lithium resource will be unable to meet the needs of people are to its.Since sodium is resourceful, and development cost is low, and sodium is with lithium
Same major element, so it is to substitute one of resource of lithium ion well.Usual lithium battery be using graphite as cathode, but
It is that, since the radius of sodium ion is larger, can not be carried out in graphite linings well reversible when graphite is for sodium-ion battery
Deintercalation, so the chemical property that it shows be not very well, capacity about 25mAh g-1.In sodium-ion battery research compared with
More carbon negative pole materials is hard carbon, and the capacity of general hard Carbon materials can about 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.]
With the raising of people's quality of life and the increase of fruit juice factory, pomace is more and more discarded, due to processing side
Formula is improper, results in a large amount of bacterial reproduction, damages to environment.At 2000 or so, pomace was once once to rivers, soil
Earth, air cause very serious pollution, and in recent years, in order to reduce harm caused by pomace, the secondary use of pomace is more next
More paid attention to by people.It but is presently mainly extensive processing mode to be carried out to it, such as animal feeding is processed into sunning, crushing
Material or fertilizer, are made wine using pomace, production jam etc..[Li Juxiu, Li Zhixi, Yang Mingquan, merchant love Juan (2002) fruit
The comprehensive utilization " Journal of Northwest Sci Tech University of Agriculture and Forestry " of slag resource, natural science edition, (z1), 103-106.].
Summary of the invention
The purpose of the present invention is to provide a kind of three-dimensional porous biomass carbon nano materials and preparation prepared using pomace
Methods and applications, this method have the characteristics that easy to operate, yield is high, low energy consumption, reproducible, the three-dimensional made from this method
The anode material of lithium-ion battery of multiporous biological matter carbon nanomaterial preparation has specific discharge capacity height, the spies such as good cycling stability
Point.
The present invention is to be achieved through the following technical solutions:
The invention discloses a kind of methods for preparing three-dimensional porous biomass carbon nano material using pomace, including following step
It is rapid:
1) by apple pomace and KOH=1:(0.3~1.5) mass ratio, take apple pomace and KOH, after mixing well, into
Row hydro-thermal reaction；
2) it after hydro-thermal reaction, is cooled to room temperature, products therefrom is heated and is concentrated, presoma is made；
3) presoma under an argon atmosphere, is warming up to 60~100 with the heating rate of 5~15 DEG C/min from room temperature
DEG C, 0.3~0.7h is kept the temperature, is then warming up to 500~900 DEG C with 5~15 DEG C/min, and keep the temperature 1.5~3.5h；
4) by product cleaning made from step 3), drying, three-dimensional porous biomass carbon nano material is made.
Step 1) the hydro-thermal reaction is after mixing well apple pomace and KOH, to be placed in reaction kettle, with 5~15
DEG C/heating rate of min, 160~200 DEG C are risen to from room temperature, keep the temperature 18~30h.
In step 3), the volume flow of argon gas is controlled in 20~100sccm.
Cleaning described in step 4) is successively to clean product deionized water and dehydrated alcohol 2~6 times.
Drying described in step 4) is at 50~90 DEG C dry 12~for 24 hours.
The invention also discloses using three-dimensional porous biomass carbon nano material made from the above method.
The invention also discloses above-mentioned three-dimensional porous biomass carbon nano materials in preparation sodium ion battery electrode material
Application.
Compared with prior art, the invention has the following beneficial technical effects:
The method disclosed by the invention for preparing three-dimensional porous biomass carbon nano material using pomace is biology using pomace
After matter source is by hydro-thermal, carbonization, the carbon nanomaterial of three-dimensional porous structure is obtained.This method is by the way that KOH, water are added in hydro-thermal
It can remove carbohydrate, solable matter in pomace when hot, also act as activation and preliminary pore-creating effect, by concentration, in turn
Tube-type atmosphere furnace carbonization is directly carried out hydrothermal product is directly concentrated after the completion of hydro-thermal, passes through without adding other pore creating materials
The rationally condition of control argon gas, is heated up with given pace and synthesizes three-dimensional porous nano carbon structure material.The method of the present invention synthesizes
Three-dimensional porous biomass carbon nano material made a big difference with traditional structure two-dimensional structure, with three-D space structure,
Biggish hole diameter allows to be easy to carry out deintercalation to provide the micro- space of sufficiently large reaction to sodium ion, and
And three-dimensional structure avoids the collapsing of its recurring structure during embedding de- well, improves the cyclical stability of material and leads
Electrically.Preparation method of the present invention is simple, and homogeneity is good, and process is easily-controllable, and the repeatability of product is high, is conducive to large-scale production.
Excellent electric conductivity, stable circulation are shown through three-dimensional porous biomass carbon nano material made from the method for the present invention
Property and high specific discharge capacity, can be widely used as anode material of lithium-ion battery.
Detailed description of the invention
Fig. 1 is the XRD diagram 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, the FESEM figure that (a) is, (b)
For HRTEM figure；
Fig. 3 is that the three-dimensional porous biomass carbon nano material of preparation is used for the cycle performance test chart of sodium-ion battery.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
A method of three-dimensional porous biomass carbon nano material is prepared using pomace, comprising the following steps:
1) preparation of presoma biomass carbon
1. weighing the apple pomace after the washed drying of 3.5g to mix with 1.05g KOH, 50ml distilled water is added in reaction
It in kettle, is sufficiently mixed, stirs；
2. rising to 160 DEG C with the heating rate of 5 DEG C/min, 18h is kept the temperature；
3. being cooled to room temperature after reaction；Product is concentrated by evaporation, biomass carbon presoma is made.
2) preparation of porous three-dimensional biomass carbon
1. the biomass carbon presoma for weighing 1g is placed in tube-type atmosphere furnace in porcelain boat, and by porcelain boat；
2. being passed through the argon gas that volume flow is 20sccm, 60 DEG C are warming up to the heating rate of 5 DEG C/min, keeps the temperature 0.7h；
3. being warming up to 500 DEG C from 60 DEG C with the heating rate of 5 DEG C/min, begin to cool after keeping the temperature 3.5h to room temperature；
4. product is cleaned 2 times with deionized water, with washes of absolute alcohol 2 times, it is dried in vacuo 12h under the conditions of 50 DEG C,
Obtain the three-dimensional porous biomass carbon of final product.
It referring to Fig. 1, can be obtained from Fig. 1, the angle 2-theta occurs " steamed bun " the shape peak of standard at 25 ° or so, can determine it
For amorphous state.
Referring to fig. 2, (a) is that the FESEM of biomass carbon schemes, it can be seen that it is three-dimensional communication structure, is had abundant
Hole configurations, aperture is about 500nm, and even size distribution, and dispersibility is preferably.(b) scheme for HRTEM, there it can be seen that
Its aperture is about 500nm, and even size distribution, and preferably, this is Na to dispersibility+Insertion and abjection provide good item
Part.
Embodiment 2
A method of three-dimensional porous biomass carbon nano material is prepared using pomace, comprising the following steps:
1) preparation of presoma biomass carbon
1. weighing the apple pomace after the washed drying of 4.5g to mix with 2.25g KOH, 50mL distilled water is added in reaction
It in kettle, is sufficiently mixed, stirs；
2. rising to 170 DEG C with the heating rate of 7 DEG C/min, 21h is kept the temperature；
3. being cooled to room temperature after reaction；Product is concentrated by evaporation, biomass carbon presoma is made.
2) preparation of porous three-dimensional biomass carbon
1. the biomass carbon presoma for weighing 2g is placed in tube-type atmosphere furnace in porcelain boat, and by porcelain boat；
2. being passed through the argon gas that volume flow is 40sccm, 70 DEG C are warming up to the heating rate of 7 DEG C/min, keeps the temperature 0.6h,
To get rid of remaining moisture in sample；
3. being warming up to 600 DEG C from 70 DEG C with the heating rate of 7 DEG C/min, begin to cool after keeping the temperature 3.0h to room temperature；
4. product is cleaned 3 times with deionized water, with washes of absolute alcohol 3 times, it is dried in vacuo 15h under the conditions of 60 DEG C,
Obtain the three-dimensional porous biomass carbon of final product.
Embodiment 3
A method of three-dimensional porous biomass carbon nano material is prepared using pomace, comprising the following steps: 1) presoma
The preparation of biomass carbon
1. weighing the apple pomace after the washed drying of 5.5g to mix with 3.85g KOH, 50ml distilled water is added in reaction
It in kettle, is sufficiently mixed, stirs；
2. rising to 180 DEG C with the heating rate of 10 DEG C/min, heat preservation is for 24 hours；
3. being cooled to room temperature after reaction；Product is concentrated by evaporation, biomass carbon presoma is made.
2) preparation of porous three-dimensional biomass carbon
1. the biomass carbon presoma for weighing 3g is placed in tube-type atmosphere furnace in porcelain boat, and by porcelain boat；
2. being passed through the argon gas that volume flow is 60sccm, 80 DEG C are warming up to the heating rate of 10 DEG C/min, keeps the temperature 0.5h,
To get rid of remaining moisture in sample；
3. being warming up to 700 DEG C from 80 DEG C with the heating rate of 10 DEG C/min, begin to cool after keeping the temperature 2.5h to room temperature；
4. product is cleaned 4 times with deionized water, with washes of absolute alcohol 4 times, it is dried in vacuo 18h under the conditions of 70 DEG C,
Obtain the three-dimensional porous biomass carbon of final product.
Embodiment 4
A method of three-dimensional porous biomass carbon nano material is prepared using pomace, comprising the following steps:
1) preparation of presoma biomass carbon
1. weighing the apple pomace after the washed drying of 6.5g to mix with 5.85g KOH, 50ml distilled water is added in reaction
It in kettle, is sufficiently mixed, stirs；
2. rising to 190 DEG C with the heating rate of 12 DEG C/min, 27h is kept the temperature；
3. being cooled to room temperature after reaction；Product is concentrated by evaporation, biomass carbon presoma is made.
2) preparation of porous three-dimensional biomass carbon
1. the biomass carbon presoma for weighing 4g is placed in tube-type atmosphere furnace in porcelain boat, and by porcelain boat；
2. being passed through the argon gas that volume flow is 80sccm, 90 DEG C are warming up to the heating rate of 12 DEG C/min, keeps the temperature 0.4h,
To get rid of remaining moisture in sample；
3. being warming up to 800 DEG C from 90 DEG C with the heating rate of 12 DEG C/min, begin to cool after keeping the temperature 2.0h to room temperature；
4. product is cleaned 5 times with deionized water, with washes of absolute alcohol 5 times, it is dried in vacuo 21h under the conditions of 80 DEG C,
Obtain the three-dimensional porous biomass carbon of final product.
Embodiment 5
A method of three-dimensional porous biomass carbon nano material is prepared using pomace, comprising the following steps:
1) preparation of presoma biomass carbon
1. weighing the apple pomace after the washed drying of 7.5g to mix with 11.25g KOH, 50ml distilled water is added in reaction
It in kettle, is sufficiently mixed, stirs；
2. rising to 200 DEG C with the heating rate of 15 DEG C/min, 30h is kept the temperature；
3. being cooled to room temperature after reaction；Product is concentrated by evaporation, biomass carbon presoma is made.
2) preparation of porous three-dimensional biomass carbon
1. the biomass carbon presoma for weighing 5g is placed in tube-type atmosphere furnace in porcelain boat, and by porcelain boat；
2. being passed through the argon gas that volume flow is 100sccm, 100 DEG C are warming up to the heating rate of 15 DEG C/min, heat preservation
0.3h, to get rid of remaining moisture in sample；
3. being warming up to 900 DEG C from 100 DEG C with the heating rate of 15 DEG C/min, begin to cool after keeping the temperature 1.5h to room temperature；
4. product is cleaned 6 times with deionized water, with washes of absolute alcohol 6 times, it is dried in vacuo for 24 hours under the conditions of 90 DEG C,
Obtain the three-dimensional porous biomass carbon of final product.
It referring to Fig. 3, can be obtained from Fig. 3, the active carbon material of three-dimensional porous structure obtained is measured in current density 100mA/g
Its reversible capacity is 335mAh/g, its capacity is still maintained at 203mAh/g after 80 circle of circulation, and coulombic efficiency is maintained at
99.0% or so, show the activated carbon from activated sludge of three-dimensional structure specific discharge capacity with higher and stable cycle performance.
In conclusion the method for the present invention mentality of designing is novel, by hydro-thermal-tube-type atmosphere furnace reaction method, and to inertia
The control of gas, the control to other factors, prepare the activated carbon from activated sludge of porous three-dimensional structure, fill to give ion
The micro- space of reaction of foot, and improve the cyclical stability of material.Simultaneously in addition, preparation process of the present invention is easily-controllable, the period is short,
The repeatability of product is high, and yield is big, is conducive to large-scale production.Through biomass active carbon made from this method for sodium ion electricity
Pond negative electrode material, which has, stablizes three-D space structure, hole configurations abundant, and its specific discharge capacity is high, cyclical stability
Well, the features such as coulombic efficiency is high.
Claims (4)
1. a kind of method for preparing three-dimensional porous biomass carbon nano material using pomace, which comprises the following steps:
1) by apple pomace and KOH=1:(0.3~1.5) mass ratio, take apple pomace and KOH, after mixing well, carry out water
Thermal response；The hydro-thermal reaction is after mixing apple pomace and KOH, distilled water to be added in reaction kettle, is sufficiently mixed, stirs
It mixes, with the heating rate of 5~15 DEG C/min, 160~200 DEG C is risen to from room temperature, keeps the temperature 18~30h；
2) it after hydro-thermal reaction, is cooled to room temperature, products therefrom is heated and is concentrated, presoma is made；
3) in the case where volume flow is the argon atmosphere of 20~100sccm, by presoma with the heating rate of 5~15 DEG C/min, certainly
Room temperature, which rises, is warming up to 60~100 DEG C, keeps the temperature 0.3~0.7h, is then warming up to 500~900 DEG C with 5~15 DEG C/min, and keep the temperature
1.5~3.5h；
4) it is dried after the deionized water of product made from step 3) and dehydrated alcohol successively being cleaned 2~6 times, three-dimensional is made
Multiporous biological matter carbon nanomaterial.
2. the method according to claim 1 for preparing three-dimensional porous biomass carbon nano material using pomace, feature exist
In, drying described in step 4) be at 50~90 DEG C dry 12~for 24 hours.
3. using three-dimensional porous biomass carbon nano material made from any one of claims 1 or 2 the method.
4. three-dimensional porous biomass carbon nano material as claimed in claim 3 answering in preparation sodium ion battery electrode material
With.
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| CN110299522B (en) * | 2019-06-26 | 2021-05-25 | 陕西科技大学 | Preparation method of fluorine-doped biomass porous carbon nano electrode material for high-capacity sodium ion battery |
| CN113200544B (en) * | 2021-04-15 | 2022-10-18 | 沈阳化工大学 | Preparation method of biomass charcoal-based supercapacitor electrode material |
| CN114477176A (en) * | 2022-01-25 | 2022-05-13 | 南京智汇环境气象产业研究院有限公司 | Apple-derived activated carbon material and preparation method thereof |
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| CN105152169A (en) * | 2015-08-11 | 2015-12-16 | 陕西科技大学 | Preparation method of biomass pomelo peel derived activated carbon serving as electrode material of super capacitor |
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