CN106784832A - A kind of preparation method of porous material and its application in sodium-ion battery - Google Patents
A kind of preparation method of porous material and its application in sodium-ion battery Download PDFInfo
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- CN106784832A CN106784832A CN201611152747.4A CN201611152747A CN106784832A CN 106784832 A CN106784832 A CN 106784832A CN 201611152747 A CN201611152747 A CN 201611152747A CN 106784832 A CN106784832 A CN 106784832A
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- Prior art keywords
- ion battery
- sodium
- porous carbon
- carbonized
- carbon materials
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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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- 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
This application discloses a kind of preparation method of porous carbon materials, it is characterised in that prepared by raw material of coffee grounds.The method raw material raw material come from twice laid, and source is sufficient, and manufacture craft is simple, for secondary utilization of resource provides new approaches；Prepared porous carbon materials show good storage sodium performance, as sodium-ion battery negative pole, with compared with high circulation stability, being a kind of cheap, environmentally safe new anode material of lithium-ion battery.
Description
Technical field
The application is related to a kind of preparation method of porous material and its application in sodium-ion battery, belongs to inorganic material
And sodium-ion battery technical field.
Background technology
With the high speed development of social economy, fossil energy resource is increasingly exhausted, changes existing irrational energy resource structure,
Greatly develop renewable and clean energy resource, it has also become the matter of utmost importance that human social faces.Lithium ion battery has
Energy density is big, have extended cycle life, operating voltage is high, memory-less effect, the advantages of self discharge is small, operating temperature range is wide, quilt
It is considered most promising green power supply, the working power and portable outfit of various electronic products has been widely used as at present
Electrokinetic cell.But, lithium ion battery is remained in several shortcomings：(1) global lithium resource is poor, increase and lithium with demand
The consumption of resource, therefore very big pressure will necessarily be produced to raw material；(2) safety issue of lithium ion battery is not yet solved
Certainly；(3) cryogenic property of lithium ion battery can not still meet actually used requirement.Therefore, finding can replace the new of lithium battery
Type energy-storage battery is particularly important.Compared with lithium resource, sodium reserves very abundant, crustal abundance is about 2.74%, and distribution is wide
General, the technology that sodium element is extracted from seawater is ripe, and the two is same major element, and chemical property is close.Sodium ion
The plurality of advantages of battery causes the study hotspot and emphasis that it turns into current green energy resource field, preceding with boundless application
Scape.
There is an obvious defect in sodium-ion battery：Sodium ion radius ratio lithium ion is big by 30%, therefore sodium ion is moved
The broader diffusion admittance of needs is moved, traditional graphite cathode material can not meet this point.At present, sodium-ion battery negative pole material
Material is mainly hard carbon.But itself once occur in it is short severe exothermic can be caused to react, the risk that set off an explosion.Additionally, hard carbon is also deposited
The problems such as discharge voltage is big with volume change.Therefore, safety economy is developed, storage sodium material of good performance turns into research heat
Point.
The content of the invention
According to the one side of the application, there is provided a kind of preparation method of porous carbon materials.The method raw material raw material come
From twice laid, source is sufficient, and manufacture craft is simple, for secondary utilization of resource provides new approaches；Prepared porous carbon
Material shows good storage sodium performance, as sodium-ion battery negative pole, with compared with high circulation stability, being that a kind of price is low
Honest and clean, environmentally safe new anode material of lithium-ion battery.
The preparation method of the porous carbon materials, it is characterised in that prepared by raw material of coffee grounds.The porous carbon
Material, is the mesoporous of 10nm~30nm containing average pore size.
As a kind of implementation method, the preparation method of the porous carbon materials, it is characterised in that at least including following step
Suddenly：
A) coffee grounds is placed in closed container, keeps being no less than 0.5 hour at 120 DEG C~200 DEG C of pre- carburizing temperature
Pre- carbonization time, obtain pre- carbonized samples；
B) step a) the pre- carbonized samples of gained are placed in alkaline solution after treatment, are washed to neutrality, obtain degreasing sample
Product；
C) after being carbonized in non-active gas atmosphere at a temperature of step b) gained degreasing samples being placed in into 600 DEG C~900 DEG C,
Obtain the porous carbon materials.
Preferably, coffee grounds before closed container is placed in, first passes through deionized water washing and dries in step a).
Preferably, pre- carburizing temperature described in step a) is 120 DEG C~180 DEG C.It is further preferred that described in step a)
Pre- carburizing temperature is 140 DEG C~160 DEG C.
Preferably, pre- carbonization time described in step a) is 0.5~5 hour.It is further preferred that pre- described in step a)
Carbonization time is 1~3 hour.
Preferably, sodium ion is contained in alkaline solution described in step b).It is further preferred that alkalescence described in step b)
Contain Na in solution2CO3And/or NaHCO3.It is further preferred that the Na described in step b) in alkaline solution2CO3And/or
NaHCO3Concentration be 0.5~5g/L.
Preferably, the pre- carbonized samples of step b) are placed in alkaline solution and are processed as stirring no less than 6 hours.Further preferably
Ground, the pre- carbonized samples of step b) are placed in alkaline solution and are processed as stirring 6 hours~10 hours.
Preferably, step c) be by step b) gained degreasing sample be placed in non-active gas atmosphere, with 1~10 DEG C/
The heating rate of min by system temperature rise to 600 DEG C~900 DEG C and keep be carbonized within 0.5~2 hour after, be cooled to room temperature,
Obtain the porous carbon materials.It is further preferred that heating rate is 5~10 DEG C/min.
Preferably, non-active gas described in step c) are selected from least one in nitrogen, inert gas.Further preferably
Ground, non-active gas described in step c) are nitrogen and/or argon gas.
As one kind preferred embodiment, the preparation method of the porous carbon materials, it is characterised in that including following step
Suddenly：
(1) clean：Appropriate coffee grounds raw material are poured into beaker, coffee grounds is carried out clearly with substantial amounts of deionized water
Wash, repeat 3~4 times, fully remove impurity that coffee grounds raw material are floated and water miscible.Coffee grounds after cleaning is positioned over
Dried in aeration cabinet stand-by；
(2) pre- carbonization：The coffee grounds that will have been dried is directly placed into the pyroreaction kettle with polytetrafluoroethyllining lining, is put
Be placed in Muffle furnace carries out pre- carbonization at 120 DEG C~200 DEG C under spontaneous pressure；
(3) degreasing：Weigh the coffee grounds after pre- carbonization to be put into beaker, soak solid with certain density alkaline solution
The fixed time, to remove remaining grease in material, the alkaline matter of residual is then washed with deionized water；
(4) it is carbonized：The coffee grounds removed after grease is put into tube furnace, programming rate, carburizing temperature, during insulation are set
Between, carry out high temperature cabonization；
(5) miniaturization grinding：Using planetary ball mill, obtain particle according to the ratio of grinding media to material ball milling for setting for a period of time
Uniform absorbent charcoal material.
Preferably, ratio of grinding media to material is 70 in the step (5):1, rotating speed is 250r/min, and Ball-milling Time is 30 minutes.
According to the another aspect of the application, there is provided a kind of anode material of lithium-ion battery, it is characterised in that contain above-mentioned
The porous carbon materials that one method is prepared.
According to the another aspect of the application, there is provided a kind of sodium-ion battery, it is characterised in that contain above-mentioned sodium-ion battery
Negative material.The sodium-ion battery include positive plate, negative plate, barrier film and electrolyte, the negative plate comprising above-mentioned sodium from
Sub- cell negative electrode material.
Preferably, the electrolyte includes organic solvent and sodium salt.It is further preferred that the sodium salt is sodium perchlorate；
The organic solvent is tetraethyleneglycol dimethyl ether.
Those skilled in the art can select suitable barrier film according to actual needs.Preferably, the barrier film is glass
Tunica fibrosa.
The beneficial effect of the application is included but is not limited to：
(1) method provided herein, raw material are recycled from discarded object, and source is sufficient, is the secondary profit of resource
With there is provided new approaches.
(2) method provided herein, manufacture craft is simple, is conducive to large-scale industrial production.
(3) method provided herein, when de-oiling fat step uses sodium carbonate and/or sodium acid carbonate, it is to avoid
Tar is formed in carbonisation, the ability of removal coffee grounds grease is improve, while being conducive to coffee carbon material loose structure
Formed.
(4) anode material of lithium-ion battery provided herein, during for sodium-ion battery, shows good storage sodium
Performance, is a kind of cheap, environmentally safe new anode material of lithium-ion battery.
Brief description of the drawings
Fig. 1 is sample 1#Stereoscan photograph.
Fig. 2 is sample 1#BJH pore size distribution curves.
Fig. 3 is battery C1#、C3#、C4#、C6#Electrochemistry cycle performance test chart.
Specific embodiment
With reference to embodiment in detail the application is described in detail, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material and apparatus in embodiments herein are bought by commercial sources.
In embodiment, the stereoscan photograph of sample is shot using the S-4800 types SEM of Hitachi, Ltd.
In embodiment, the duct of sample uses the Asap2020HD88 type specific surface area and porosity analyzers of Merck ＆ Co., Inc
Device is determined.
In embodiment, the LAND battery test systems of the electric property of battery in Lan Bo test equipments Co., Ltd of Wuhan City
Upper measure.
The sample 1 of embodiment 1#~6#Preparation
Comprise the following steps that：
(1) clean：100g coffee grounds raw material are poured into beaker, coffee grounds is cleaned with 500mL deionized waters,
It is repeated 3 times, fully removes impurity that coffee grounds raw material are floated and water miscible.Coffee grounds after cleaning is positioned over ventilation dry
It is stand-by in 120 DEG C of drying in dry case；
(2) pre- carbonization：The coffee grounds that will have been dried is directly placed into the pyroreaction kettle with polytetrafluoroethyllining lining, is put
It is placed in Muffle furnace in pre- carbonization a period of time under pre- carburizing temperature, spontaneous pressure；
(3) degreasing：Weigh the coffee grounds 5g after pre- carbonization to be put into beaker, with the alkaline solution of 250mL, at room temperature
Immersion a period of time, continuously stirred by magnetic stirring apparatus, to remove remaining grease in material, then cleaned with deionized water
Fall the alkaline matter of residual；
(4) it is carbonized：The coffee grounds removed after grease is put into tube furnace, non-active gas are passed through, programming rate is set,
Carburizing temperature and soaking time, high temperature are carbonized；
(5) miniaturization grinding, using planetary ball mill, according to the ratio of grinding media to material 70 of setting:1, rotating speed is 250r/min, ball
It is 30 minutes to consume time, and obtains evengranular porous carbon material.
Sample number into spectrum, raw material, preparation condition refer to table 1.
Table 1
The sample 1 of embodiment 2#~6#Sign
Using stereoscan photograph to sample 1#~6#Pattern before miniaturization grinding is detected that testing result shows, sample
Product 1#~6#It is block lamellar structure before miniaturization grinding, the size of fragment is generally 1~2 μm.Typical Representative is sample 1#,
Its electromicroscopic photograph is as shown in Figure 1.
To sample 1#~6#Specific surface area and aperture be determined, as a result show, sample 1#~6#Specific surface integration
Cloth is in 93~96m2Between/g, average pore size is distributed between 10nm~30nm.Typical Representative is sample 1#, its BJH pore-size distribution
Curve is as shown in Figure 2.
The battery C1 of embodiment 3#~C6#Making
Negative plate N1#~N6#Preparation
Respectively with sample 1#~sample 6#As negative material, negative plate is prepared, comprised the following steps that：
Negative material, conductive agent conductive black, bonding agent polyvinylidene fluoride are mixed in 1-METHYLPYRROLIDONE
It is even, it is made cathode size.Comprising 70% negative active core-shell material, 20% conductive black, 10% in its slurry solids composition
Polyvinylidene fluoride.Cathode size is uniformly coated on the negative current collector Copper Foil that thickness is 20 μm, then at 85 DEG C
Cut into slices after drying, compressing tablet, weighed, obtained final product negative plate.Respectively with sample 1#~sample 6#As negative material, prepare
Negative plate, N1 is designated as respectively#~N6#。
The preparation of electrolyte
To sodium perchlorate is added in tetraethyleneglycol dimethyl ether, the solution that sodium perchlorate concentration is 1mol/L, as electricity are obtained
Solution liquid.
Sodium ion secondary battery C1#~C6#Preparation
Using glass fibre membrane as barrier film.
Using metallic sodium as positive plate, (water content and oxygen content are respectively less than 1ppm) assembling in the glove box full of argon gas
Half-cell.
Respectively with N1#~N6#The sodium-ion battery prepared as negative plate, is designated as battery C1 respectively#~battery C6#。
The battery C1 of embodiment 4#~battery C9#Specific capacity test
Respectively to the battery C1 of preparation in embodiment 3#(700 DEG C), battery C3#(600 DEG C), battery C4#(800 DEG C) and electricity
Pond C6#The specific capacity of (900 DEG C) is tested, and is concretely comprised the following steps：
At 25 DEG C, 0.01V is discharged to according to certain discharge current；After electric discharge terminates, battery standing 5 minutes；Then
With certain current density constant-current charge to 3.0V, after charging terminates, battery standing is after 5 minutes with identical current density constant current
It is discharged to 0.01V；Battery stands 5 minutes after completely filling, then is charged with identical condition.
The preceding current density of charge and discharge cycles twice is 50mA/g, and negative electrode is activated with low current density, is formed
More the SEI films of even compact, are then circulated performance test under the current density of 200mA/g.With battery 1#As a example by, its
Discharge capacity is 362.6mAh/g first, and the second circle cyclic discharge capacity is 168.1mAh/g, and after 50 circle circulations, capacity still keeps
In 91.7% (see Fig. 3) of the second circle.
As seen from Figure 3, using the porous carbon materials of herein described method preparation as sodium-ion battery negative pole material
Cycle charge-discharge specific capacity keeps preferable during material, stable cycle performance.
The announcement of book according to the above description, the application those skilled in the art can also be carried out to above-mentioned implementation method
Appropriate change and modification.Therefore, the application is not limited to specific embodiment disclosed and described above, to the application's
Some modifications and changes should also be as falling into the protection domain of claims hereof.
Claims (10)
1. a kind of preparation method of porous carbon materials, it is characterised in that prepared by raw material of coffee grounds.
2. method according to claim 1, it is characterised in that at least comprise the following steps：
A) coffee grounds is placed in closed container, keeps pre- no less than 0.5 hour at 120 DEG C~200 DEG C of pre- carburizing temperature
Carbonization time, obtains pre- carbonized samples；
B) step a) the pre- carbonized samples of gained are placed in alkaline solution after treatment, are washed to neutrality, obtain degreasing sample；
C) after being carbonized in non-active gas atmosphere at a temperature of step b) gained degreasing samples being placed in into 600 DEG C~900 DEG C, obtain final product
To the porous carbon materials.
3. method according to claim 1, it is characterised in that coffee grounds is first passed through before closed container is placed in step a)
Cross deionized water washing and dry.
4. method according to claim 1, it is characterised in that pre- carburizing temperature described in step a) is 120 DEG C~180
℃；Preferably, pre- carburizing temperature described in step a) is 140 DEG C~160 DEG C；
Pre- carbonization time described in step a) is 0.5~5 hour；Preferably, pre- carbonization time described in step a) is 1~3 small
When.
5. method according to claim 1, it is characterised in that contain sodium ion in alkaline solution described in step b)；It is excellent
Selection of land, Na is contained described in step b) in alkaline solution2CO3And/or NaHCO3。
6. method according to claim 1, it is characterised in that the pre- carbonized samples of step b) are placed in alkaline solution and are processed as
Stirring is no less than 6 hours；Preferably, the pre- carbonized samples of step b) are placed in alkaline solution and are processed as stirring 6 hours~10 hours.
7. method according to claim 1, it is characterised in that step c) be step b) gained degreasing samples are placed in it is non-
In reactive gas atmosphere, system temperature is risen to by 600 DEG C~900 DEG C and holding 0.5~3 with the heating rate of 1~10 DEG C/min
After hour is carbonized, room temperature is cooled to, that is, obtains the porous carbon materials.
8. the method according to claim 1 or 7, it is characterised in that non-active gas described in step c) are selected from nitrogen, lazy
At least one in property gas.
9. a kind of anode material of lithium-ion battery, it is characterised in that be prepared into containing with good grounds any one of claim 1 to 8 method
The porous carbon materials for arriving.
10. a kind of sodium-ion battery, it is characterised in that contain the anode material of lithium-ion battery described in claim 9.
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Cited By (2)
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| CN107892300A (en) * | 2017-11-15 | 2018-04-10 | 广东环境保护工程职业学院 | A kind of coffee grounds valuable component separation and recovery method and application |
| CN111204731A (en) * | 2020-01-07 | 2020-05-29 | 大连理工大学 | Preparation method of hard carbon negative electrode material of sodium ion battery |
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