CN106744790A - A kind of biological carbon electrode material and preparation method thereof - Google Patents
A kind of biological carbon electrode material and preparation method thereof Download PDFInfo
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- CN106744790A CN106744790A CN201611073358.2A CN201611073358A CN106744790A CN 106744790 A CN106744790 A CN 106744790A CN 201611073358 A CN201611073358 A CN 201611073358A CN 106744790 A CN106744790 A CN 106744790A
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
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Abstract
The present invention relates to a kind of biological carbon electrode material and preparation method thereof, first straw is mixed with water and ball milling is carried out, obtain plant straw powder；Wherein the ratio of straw and water is 3g：(20~50) mL；Again to activator is added in the plant straw powder after ball milling, then under the protection of protective gas, it is warming up to 500~1100 DEG C and is incubated 2~6h；The product postprocessing after insulation is finally obtained into biological carbon electrode material.The present invention prepares biological carbon electrode material using reproducible agricultural by-products straw, and by ball milling, activator carbonization is obtained the tridimensional network carbon material with certain degree of graphitization；Obtained material is a kind of three dimensional network structure, with good ion insertion and diffusion, shortens insertion and the abjection distance of ion, it is ensured that the cyclical stability of sodium-ion battery.
Description
【Technical field】
The invention belongs to electrode material preparing technical field, and in particular to a kind of biological carbon electrode material and its preparation side
Method.
【Background technology】
Battery i.e. electrochemical cell, are that chemical energy is stored as into electric energy, or because electrochemical reaction produces electric current.Battery
Main Types can be divided into two kinds, including galvanic cell and battery.During galvanic cell storage of chemical energy, only when battery is put completely
Can not be used again after electric.For battery, potential during current work is higher than cell voltage potential, and now occurring can
Inverse redox reaction, battery can repeatedly discharge and recharge.Nowadays, the life of people increasingly be unable to do without battery, such as
Notebook computer used in everyday, mobile communication, electric automobile and intelligent grid etc., usually with battery as energy storage device.
Lithium ion battery and sodium-ion battery belong to battery, i.e. secondary cell.Lithium ion cell positive generally uses cobalt acid lithium, manganese
Sour lithium, LiFePO 4 etc., negative pole is generally using native graphite, carbonaceous mesophase spherules, needle coke, resin carbon, biomass carbon etc.
Carbon material.Lithium ion battery has that energy density is high, has extended cycle life, operating voltage is high, memory-less effect, self discharge are small, work
Make the unrivaled advantages such as temperature range is wide, environment-friendly, safe.
With the progress and development in epoch, people are more and more urgent for the demand of the energy.Nowadays electric automobile, wind
Energy, the exploitation of solar energy, the requirement for energy storage device are also improved constantly.Due to the skewness of elemental lithium, no
Easily exploitation, and price, lithium ion battery is far from the demand for meeting contemporary people.For the sodium with lithium with main group, its
Rich reserves, it is cheap and easy to get, therefore, sodium-ion battery obtains the concern of people again.Lithium and sodium belong to same major element, have
Similar physics and chemical property, but different radius sizes so that the negative material for being applied to lithium ion battery can not be complete
The full sodium suitable for large-size.
Biomass are a kind of cleaning and reproducible resource, in resource and environmental problem increasingly serious today, exploitation and
There is great strategic importance using biomass resource.Rape shell is the byproduct of crops rapeseed product, aboundresources, oil
Dish shell has excellent natural structure, understands that carbon content reaches 53% by analyzing its composition, but, big portion very low currently with rate
It is allocated as being abandoned for waste or is utilized as inferior fuel.
【The content of the invention】
It is an object of the invention to overcome problems of the prior art, there is provided a kind of biological carbon electrode material and its system
Preparation Method, by the use of straw as raw material, obtained material can be used as the negative material of sodium-ion battery.
In order to achieve the above object, the inventive method is adopted the following technical scheme that：
Comprise the following steps：
(1) straw is mixed with water and carries out ball milling, obtain plant straw powder；The ratio of wherein straw and water is
3g：(20~50) mL；
(2) to activator is added in the plant straw powder after ball milling, then under the protection of protective gas, 500 are warming up to
~1100 DEG C and 2~6h of insulation；
(3) product postprocessing after insulation is obtained into biological carbon electrode material.
Further, the rotational speed of ball-mill in step (1) is 300~500r/min.
Further, the Ball-milling Time in step (1) is 1~2h.
Further, activator is KOH, NaOH, ZnCl in step (2)2、K2CO3Or MgO.
Further, activator and the mass ratio of plant straw powder are (0.5~3) in step (2)：1.
Further, protective gas is one or any two kinds in nitrogen, argon gas, helium and neon in step (2)
Mixed gas above, the flow velocity of protective gas is 20sccm~100sccm.
Further, the heating rate in step (2) is 1~10 DEG C/min.
Further, the post processing in step (3) is to wash the product after insulation with hydrochloric acid, deionized water and ethanol successively
Wash to neutrality, then be vacuum dried 12~24h.
Biological carbon electrode material obtained in a kind of preparation method using biology carbon electrode material as described above.
Compared with prior art, the present invention has following beneficial technique effect：
Biological carbon electrode material is prepared using reproducible agricultural by-products straw in the inventive method, by ball
Mill, activator carbonization, is obtained the tridimensional network carbon material with certain degree of graphitization.The method preparation process is simple,
Low cost, the impurity element that straw contains in itself is less, and impurity removal process is simple, prepares the few purity of impurity in products high；It is obtained
Material be a kind of three dimensional network structure, with good ion insertion and diffusion, it is ensured that the circulation of sodium-ion battery
Stability.The present invention utilizes the straw classes such as rape stalk, maize straw, rice husk, rape shell, straw, cotton stalk biological
Matter raw material replaces timber to prepare new carbon electrode material with plastics, can make full use of abandoned biomass resource, it is to avoid directly burn
When caused environmental pollution, for it provides an approach for reliable sustainable development, also for the preparation of carbon electrode material is carried
New path is supplied.
Carbon electrode material of the present invention is tridimensional network, shortens insertion and the abjection distance of ion, and with big ratio
Surface area, the sodium-ion battery of assembling has excellent chemical property, in 100mA g-1Capacity is maintained under current density
90mAh g-1。
【Brief description of the drawings】
Fig. 1 schemes to prepare the SEM of carbon material in the embodiment of the present invention 1.
Fig. 2 (a) is the N adsorption/desorption curves of the carbon material of preparation in embodiments of the invention 1, and Fig. 2 (b) is of the invention
The pore size distribution curve of the carbon material prepared in embodiment 1.
Fig. 3 (a) is the cycle performance curve map of the carbon material of preparation in embodiments of the invention 1, and Fig. 3 (b) is the present invention
Embodiment 1 in prepare carbon material high rate performance curve map.
【Specific embodiment】
The present invention is described in further details below in conjunction with the accompanying drawings.
Straw uses rape stalk, maize straw, rice husk, rape shell, straw or cotton stalk in the present invention；At it
Reason mode is identical, is illustrated by taking rape shell as an example below, a kind of preparation side of network structure biology carbon electrode material of the invention
Method, including following steps：
First, the rape shell after every 3g washing dryings are shredded mixes with the water of 20~50mL；300~500r/min's
1~2h of ball milling under rotating speed, it is (0.5~3) that activator is pressed after drying with the mass ratio of the rape shell crushed：1 adds activator, living
Agent can be KOH, NaOH, ZnCl2, K2CO3, any one in MgO；It is transferred under atmosphere furnace, by liter under atmosphere protection
Warm speed is warmed up to design temperature for 1~10 DEG C/min, such as 500~1100 DEG C 2~6h of insulation；Wherein protective gas be nitrogen,
Any one in argon gas, helium, neon or two or more mixed gas, gas flow rate are 20sccm~100sccm；Again
6~24h of magnetic agitation at room temperature is added in the hydrochloric acid of 3mol/L, deactivator is removed to wash；Finally use deionized water and second
Alcohol is washed 3 times, and 12~24h of vacuum drying obtains skeletal porous carbon electrode material.
Embodiment one：
Rape shell after 3g washing dryings are shredded mixes with 20ml water；The ball milling 2h under the rotating speed of 300r/min, dries
KOH and rape shell are mixed with 1 ratio afterwards, are transferred under atmosphere furnace, protect lower 5 DEG C/min to heat up in argon gas atmosphere (50sccm)
To 800 DEG C of insulation 2h；Again with magnetic agitation 12h under 3mol/L hydrochloric acid normal temperature；Finally wash 3 times with deionized water and ethanol, very
Sky dries 12h and obtains network-like structure biology carbon electrode material.
From figure 1 it appears that prepared carbon material is tridimensional network；
As can be seen that prepared carbon material has big specific surface area 673.5m from Fig. 2 (a)2g-1；Can from Fig. 2 (b)
To find out, pore-size distribution is in 30-50nm；
The sodium-ion battery of carbon electrode material assembling has excellent chemical property.From Fig. 3 (a) cycle performance curves
In as can be seen that in 100mA g-1Capacity maintains 90mAh g under current density-1；Can be with from Fig. 3 (b) high rate performance curves
Find out, 50,100,200 500,1000,2000 and 5000m A g-1Under current density, capacity is 130,92,70,61,52,
45 and 30mAh g-1, when current density returns to 50m A g-1, capacity restoration to 130mAh g-1.Its chemical property is attributed to it
Unique tridimensional network, shortens insertion and the abjection distance of ion.
Embodiment two：
Rape shell after 3g washing dryings are shredded mixes with 30ml water；The ball milling 2h under the rotating speed of 500r/min, dries
KOH and rape shell are mixed with 3 ratio afterwards, are transferred under atmosphere furnace, and lower 5 DEG C/min liters are protected in neon atmosphere (100sccm)
Temperature is incubated 2h to 1000 DEG C；Again with magnetic agitation 12h under 3mol/L hydrochloric acid normal temperature；Finally washed 3 times with deionized water and ethanol,
Vacuum drying 24h obtains network-like structure biology carbon electrode material.
Embodiment three：
Rape shell after 3g washing dryings are shredded mixes with 50ml water；The ball milling 2h under the rotating speed of 300r/min, dries
K afterwards2CO3Mixed with 1 ratio with rape shell, be transferred under atmosphere furnace, lower 1 DEG C/min liters are protected in nitrogen atmosphere (20sccm)
Temperature is incubated 6h to 500 DEG C；Again with magnetic agitation 24h under 3mol/L hydrochloric acid normal temperature；Finally washed 3 times with deionized water and ethanol,
Vacuum drying 18h obtains network-like structure biology carbon electrode material.
Example IV：
Rape shell after 3g washing dryings are shredded mixes with 20ml water；The ball milling 2h under the rotating speed of 500r/min, dries
Post activation agent (KOH:K2CO3=1) mixed with 0.5 ratio with rape shell, it is transferred under atmosphere furnace, in argon gas atmosphere
900 DEG C of insulation 5h are warmed up to 10 DEG C/min under (100sccm) protection；Again with magnetic agitation 6h under 3mol/L hydrochloric acid normal temperature；Most
Washed 3 times with deionized water and ethanol afterwards, vacuum drying 12h obtains network-like structure biology carbon electrode material.
Embodiment five：
Rape shell after 3g washing dryings are shredded mixes with 20ml water；The ball milling 2h under the rotating speed of 300r/min, dries
MgO and rape shell are mixed with 1 ratio afterwards, are transferred under atmosphere furnace, and lower 5 DEG C/min liters are protected in argon gas atmosphere (100sccm)
Temperature is incubated 2h to 1100 DEG C；Again with magnetic agitation 10h under 3mol/L hydrochloric acid normal temperature；Finally washed 3 times with deionized water and ethanol,
Vacuum drying 24h obtains network-like structure biology carbon electrode material.
The present invention relates to the preparation method of sodium-ion battery biology carbon electrode material, using reproducible agricultural by-products oil
Dish shell prepares biological carbon electrode material, and preparation process is simple, low cost, obtained material electrochemical performance are excellent, are a kind of nets
Shape rape shell base biology carbon electrode material.The present invention has advantages below：
(1) impurity element that raw material rape shell of the invention contains in itself is less, and impurity removal process is simple, prepares impurity in products
Few purity is high.
(2) the network structure biology carbon electrode material that prepared by the present invention has three-dimensional structure, it is ensured that the circulation of battery is steady
It is qualitative.
(3) preparation process is simple of the invention, easy industrialized production.
This discarded biomass of rape shell are changed into carbon electrode by the present invention, are a kind of agricultures for meeting circular economy concept
Woods fixed-end forces mode, obtained material is the Suitable base for preparing carbon electrode.
Claims (9)
1. a kind of preparation method of biological carbon electrode material, it is characterised in that：Comprise the following steps：
(1) straw is mixed with water and carries out ball milling, obtain plant straw powder；Wherein the ratio of straw and water is 3g：
(20~50) mL；
(2) to activator is added in the plant straw powder after ball milling, then under the protection of protective gas, it is warming up to 500~
1100 DEG C and 2~6h of insulation；
(3) product postprocessing after insulation is obtained into biological carbon electrode material.
2. the preparation method of a kind of biological carbon electrode material according to claim 1, it is characterised in that：In step (1)
Rotational speed of ball-mill is 300~500r/min.
3. the preparation method of a kind of biological carbon electrode material according to claim 1, it is characterised in that：In step (1)
Ball-milling Time is 1~2h.
4. the preparation method of a kind of biological carbon electrode material according to claim 1, it is characterised in that：It is living in step (2)
Agent is KOH, NaOH, ZnCl2、K2CO3Or MgO.
5. the preparation method of a kind of biological carbon electrode material according to claim 1, it is characterised in that：It is living in step (2)
Agent is (0.5~3) with the mass ratio of plant straw powder：1.
6. the preparation method of a kind of biological carbon electrode material according to claim 1, it is characterised in that：Protected in step (2)
Shield gas is the one or any two or more mixed gas in nitrogen, argon gas, helium and neon, the flow velocity of protective gas
It is 20sccm~100sccm.
7. the preparation method of a kind of biological carbon electrode material according to claim 1, it is characterised in that：In step (2)
Heating rate is 1~10 DEG C/min.
8. the preparation method of a kind of biological carbon electrode material according to claim 1, it is characterised in that：In step (3)
Post processing is to wash to neutrality the product after insulation with hydrochloric acid, deionized water and ethanol successively, then is vacuum dried 12~24h.
9. biological carbon electrode material obtained in the preparation method of biological carbon electrode material described in a kind of utilization claim 1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107681230A (en) * | 2017-08-18 | 2018-02-09 | 中国科学院合肥物质科学研究院 | A kind of zinc-air battery and its application |
| CN109546139A (en) * | 2019-01-07 | 2019-03-29 | 合肥学院 | A kind of metal sulfide/carbon composite, preparation method and its application in cell negative electrode material |
| CN109796004A (en) * | 2019-03-26 | 2019-05-24 | 成都大学 | A kind of lithium cell cathode material and preparation method thereof and the lithium battery comprising the negative electrode material |
| CN110316714A (en) * | 2019-06-17 | 2019-10-11 | 西安交通大学苏州研究院 | Three-dimensional porous class graphene structural carbon material based on rice husk and its preparation method and application |
| CN112624111A (en) * | 2021-01-13 | 2021-04-09 | 齐鲁工业大学 | Preparation method of metal-catalyzed corn straw derived carbon electrode material |
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| CN109546139A (en) * | 2019-01-07 | 2019-03-29 | 合肥学院 | A kind of metal sulfide/carbon composite, preparation method and its application in cell negative electrode material |
| CN109796004A (en) * | 2019-03-26 | 2019-05-24 | 成都大学 | A kind of lithium cell cathode material and preparation method thereof and the lithium battery comprising the negative electrode material |
| CN110316714A (en) * | 2019-06-17 | 2019-10-11 | 西安交通大学苏州研究院 | Three-dimensional porous class graphene structural carbon material based on rice husk and its preparation method and application |
| CN112624111A (en) * | 2021-01-13 | 2021-04-09 | 齐鲁工业大学 | Preparation method of metal-catalyzed corn straw derived carbon electrode material |
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