CN106784832B - 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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- CN106784832B CN106784832B CN201611152747.4A CN201611152747A CN106784832B CN 106784832 B CN106784832 B CN 106784832B CN 201611152747 A CN201611152747 A CN 201611152747A CN 106784832 B CN106784832 B CN 106784832B
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- porous carbon
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- ion battery
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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 methods of porous carbon materials, which is characterized in that is prepared by raw material of coffee grounds.This method raw material raw material come from waste utilization, and source is sufficient, and manufacture craft is simple, provides new approaches for the secondary use of resource；Prepared porous carbon materials show good storage sodium performance, are used as sodium-ion battery cathode, have compared with high circulation stability, are a kind of cheap, novel anode material of lithium-ion batteries of no pollution to the environment.
Description
Technical field
Application this application involves a kind of preparation method of porous material and its in sodium-ion battery, belongs to inorganic material
And sodium-ion battery technical field.
Background technique
With the high speed development of social economy, fossil energy resource is increasingly exhausted, changes existing unreasonable 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, has extended cycle life, operating voltage height, memory-less effect, the advantages that self discharge is small, operating temperature range is wide, quilt
It is considered most promising green power supply, has been widely used as the working power and portable outfit of various electronic products at present
Power battery.But lithium ion battery still has several disadvantages: (1) global lithium resource is poor, increase and lithium with demand
The consumption of resource, therefore very big pressure will necessarily be generated to raw material；(2) safety issue of lithium ion battery not yet solves
Certainly；(3) cryogenic property of lithium ion battery is not able to satisfy the requirement of actual use still.Therefore, the new of lithium battery can be replaced by finding
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 mature, and the two is same major element, and chemical property is close.Sodium ion
The plurality of advantages of battery causes it to become the research hotspot and emphasis in current green energy resource field, before boundless application
Scape.
There are an apparent defects for sodium-ion battery: sodium ion radius ratio lithium ion is big by 30%, therefore sodium ion moves
It moves and needs broader diffusion admittance, traditional graphite cathode material is not able to satisfy this point.Currently, sodium-ion battery cathode material
Material is mainly hard carbon.But the interior short risk that severe exothermic can be caused to react, set off an explosion that once it occur.In addition, 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 becomes research heat
Point.
Summary of the invention
According to the one aspect of the application, a kind of preparation method of porous carbon materials is provided.This method raw material raw material come
From waste utilization, source is sufficient, and manufacture craft is simple, provides new approaches for the secondary use of resource；Prepared porous carbon
Material shows good storage sodium performance, is used as sodium-ion battery cathode, has compared with high circulation stability, is that a kind of price is low
It is honest and clean, the novel anode material of lithium-ion battery of no pollution to the environment.
The preparation method of the porous carbon materials, which is characterized in that be prepared by raw material of coffee grounds.The porous carbon
Material is the mesoporous of 10nm~30nm containing average pore size.
As an implementation, the preparation method of the porous carbon materials, which is characterized in that include at least following step
It is rapid:
A) coffee grounds is placed in closed container, is kept at 120 DEG C~200 DEG C of pre- carburizing temperature no less than 0.5 hour
Pre- carbonization time, obtain pre- carbonized samples；
B) pre- carbonized samples obtained by step a) are placed in alkaline solution after handling, wash to neutrality, obtains degreasing sample
Product；
C) after being carbonized in non-active gas atmosphere at a temperature of degreasing sample obtained by step b) being placed in 600 DEG C~900 DEG C,
Obtain the porous carbon materials.
Preferably, coffee grounds first passes through deionized water washing and drying before being placed in closed container 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, contain sodium ion in alkaline solution described in step b).It is further preferred that alkalinity described in step b)
Contain Na in solution2CO3And/or NaHCO3.It is further preferred that the Na in alkaline solution described in step b)2CO3And/or
NaHCO3Concentration be 0.5~5g/L.
Preferably, it is stirring no less than 6 hours that the pre- carbonized samples of step b), which are placed in processing in alkaline solution,.Further preferably
Ground, it is stirring 6 hours~10 hours that the pre- carbonized samples of step b), which are placed in processing in alkaline solution,.
Preferably, step c) is that degreasing sample obtained by step b) is placed in non-active gas atmosphere, with 1~10 DEG C/
System temperature is risen to 600 DEG C~900 DEG C and is kept for 0.5~2 hour after being carbonized by the heating rate of min, is 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) is selected from least one of nitrogen, inert gas.Further preferably
Ground, non-active gas described in step c) are nitrogen and/or argon gas.
As a preferred embodiment, the preparation method of the porous carbon materials, which is characterized in that including following step
It is rapid:
(1) it cleans: appropriate coffee grounds raw material being poured into beaker, coffee grounds is carried out clearly with a large amount of deionized water
It washes, repeats 3~4 times, sufficiently remove impurity that coffee grounds raw material float and water-soluble.Coffee grounds after cleaning is placed in
It is dried in aeration cabinet stand-by；
(2) pre- carbonization: the coffee grounds dried is directly placed into the pyroreaction kettle with polytetrafluoroethyllining lining, is put
It is placed in Muffle furnace and is carbonized in advance under spontaneous pressure at 120 DEG C~200 DEG C；
(3) degreasing: weighing the coffee grounds after pre- carbonization and be put into beaker, is impregnated with certain density alkaline solution solid
Then the fixed time washes remaining alkaline matter with deionized water to remove remaining grease in material；
(4) it is carbonized: the coffee grounds after grease will be removed and be put into tube furnace, heating rate, carburizing temperature, when heat preservation are set
Between, carry out high temperature cabonization；
(5) miniaturization grinding: use planetary ball mill, according to setting ratio of grinding media to material ball milling for a period of time, obtain particle
Uniform absorbent charcoal material.
Preferably, ratio of grinding media to material is 70:1 in the step (5), and revolving speed 250r/min, Ball-milling Time is 30 minutes.
According to the another aspect of the application, a kind of anode material of lithium-ion battery is provided, which is characterized in that contain above-mentioned
The porous carbon materials that one method is prepared.
According to the another aspect of the application, a kind of sodium-ion battery is provided, which is characterized in that contain above-mentioned sodium-ion battery
Negative electrode material.The sodium-ion battery includes positive plate, negative electrode tab, diaphragm and electrolyte, the negative electrode tab include 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 isolation film according to actual needs.Preferably, the isolation film is glass
Tunica fibrosa.
The beneficial effect of the application includes but is not limited to:
(1) method provided herein, raw material are recycled from waste, and source is sufficient, are the secondary benefit of resource
With providing new approaches.
(2) method provided herein, manufacture craft is simple, is conducive to large-scale industrial production.
(3) method provided herein is avoided when de-oiling rouge step uses sodium carbonate and/or sodium bicarbonate
Tar is formed in carbonisation, improves the ability of removal coffee grounds grease, while being conducive to coffee carbon material porous structure
It is formed.
(4) anode material of lithium-ion battery provided herein shows good storage sodium when being used for sodium-ion battery
Performance is a kind of cheap, novel anode material of lithium-ion battery of no pollution to the environment.
Detailed description of the invention
Fig. 1 is sample 1#Stereoscan photograph.
Fig. 2 is sample 1#BJH pore size distribution curve.
Fig. 3 is battery C1#、C3#、C4#、C6#Electrochemistry cycle performance test chart.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material in embodiments herein and instrument are bought by commercial sources.
In embodiment, the stereoscan photograph of sample is shot using the S-4800 type scanning electron microscope of Hitachi, Ltd.
In embodiment, the duct of sample uses the Asap2020HD88 type specific surface area and porosity analyzer of Merck & Co., Inc
Device measurement.
In embodiment, the LAND battery test system of the electric property of battery in Lan Bo test equipment Co., Ltd, Wuhan City
Upper measurement.
1 sample 1 of embodiment#~6#Preparation
Specific step is as follows:
(1) it cleans: 100g coffee grounds raw material being poured into beaker, coffee grounds is cleaned with 500mL deionized water,
It is repeated 3 times, sufficiently removes impurity that coffee grounds raw material float and water-soluble.It is dry that coffee grounds after cleaning is placed in ventilation
It is stand-by in 120 DEG C of drying in dry case；
(2) pre- carbonization: the coffee grounds dried is directly placed into the pyroreaction kettle with polytetrafluoroethyllining lining, is put
In advance carbonization a period of time is placed in Muffle furnace under pre- carburizing temperature, spontaneous pressure；
(3) degreasing: weighing the coffee grounds 5g after pre- carbonization and be put into beaker, with the alkaline solution of 250mL, at room temperature
It is soaked for a period of time, is continuously stirred by magnetic stirring apparatus, to remove remaining grease in material, then cleaned with deionized water
Fall remaining alkaline matter；
(4) it is carbonized: the coffee grounds after removal grease being put into tube furnace, non-active gas is passed through, heating 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 70:1 of setting, revolving speed 250r/min, ball
Time consuming is 30 minutes, obtains evengranular porous carbon material.
See Table 1 for details for sample number into spectrum, raw material, preparation condition.
Table 1
2 sample 1 of embodiment#~6#Characterization
Using stereoscan photograph to sample 1#~6#Pattern before miniaturization grinding is detected, and testing result is shown, sample
Product 1#~6#It is blocky lamellar structure before miniaturization grinding, the size of fragment is mostly 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, the results show that sample 1#~6#Specific surface integral
Cloth is in 93~96m2Between/g, average pore size is distributed between 10nm~30nm.Typical Representative is sample 1#, BJH pore-size distribution
Curve is as shown in Figure 2.
3 battery C1 of embodiment#~C6#Production
Negative electrode tab N1#~N6#Preparation
Respectively with sample 1#~sample 6#As negative electrode material, negative electrode tab is prepared, the specific steps are as follows:
Negative electrode material, conductive agent conductive black, bonding agent polyvinylidene fluoride are mixed in N-Methyl pyrrolidone
It is even, negative electrode slurry is made.It include 70% negative electrode active material, 20% conductive black, 10% in its slurry solids ingredient
Polyvinylidene fluoride.Negative electrode slurry is uniformly coated on the negative current collector copper foil with a thickness of 20 μm, then at 85 DEG C
It is sliced after drying, tabletting, weighing is to get negative electrode tab.Respectively with sample 1#~sample 6#As negative electrode material, it is prepared
Negative electrode tab, be denoted as N1 respectively#~N6#。
The preparation of electrolyte
Sodium perchlorate is added into tetraethyleneglycol dimethyl ether, obtains the solution that sodium perchlorate concentration is 1mol/L, it is as electric
Solve liquid.
Sodium ion secondary battery C1#~C6#Preparation
Using glass fibre membrane as diaphragm.
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#As the sodium-ion battery that negative electrode tab is prepared, it is denoted as battery C1 respectively#~battery C6#。
4 battery C1 of embodiment#~battery C9#Specific capacity test
Respectively to the battery C1 prepared 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, specific steps are as follows:
At 25 DEG C, 0.01V is discharged to according to certain discharge current；After electric discharge, battery standing 5 minutes；Then
With certain current density constant-current charge to 3.0V, after charging, battery standing is after five minutes with identical current density constant current
It is discharged to 0.01V；Battery stands 5 minutes after completely filling, then with the charging of identical condition.
The preceding current density of charge and discharge cycles twice is 50mA/g, is activated with low current density to negative electrode, is formed
Then the more SEI film of even compact carries out cycle performance test under the current density of 200mA/g.With battery 1#For,
Discharge capacity is 362.6mAh/g for the first time, and the second circle cyclic discharge capacity is 168.1mAh/g, and after 50 circles recycle, capacity is still kept
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 cathode material
Cycle charge-discharge specific capacity is kept preferably when material, stable cycle performance.
The announcement of book according to the above description, the application those skilled in the art can also carry out above embodiment
Change and modification appropriate.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 scope of claims hereof.
Claims (12)
1. a kind of preparation method of porous carbon materials, which is characterized in that be prepared, include at least following by raw material of coffee grounds
Step:
A) coffee grounds is placed in closed container, no less than 0.5 hour pre- is kept at 120 DEG C~200 DEG C of pre- carburizing temperature
Carbonization time obtains pre- carbonized samples；
B) pre- carbonized samples obtained by step a) are placed in alkaline solution after handling, wash to neutrality, obtains degreasing sample；
C) after being carbonized in non-active gas atmosphere at a temperature of degreasing sample obtained by step b) being placed in 600 DEG C~900 DEG C to get
To the porous carbon materials；
It is the mesoporous of 10~30nm that the porous carbon materials, which contain average pore size,.
2. the method according to claim 1, wherein coffee grounds first passes through before being placed in closed container in step a)
Cross deionized water washing and drying.
3. the method according to claim 1, wherein pre- carburizing temperature described in step a) is 120 DEG C~180
℃；
Pre- carbonization time described in step a) is 0.5~5 hour.
4. according to the method described in claim 3, it is characterized in that, pre- carburizing temperature described in step a) is 140 DEG C~160
℃；Pre- carbonization time described in step a) is 1~3 hour.
5. the method according to claim 1, wherein containing sodium ion in alkaline solution described in step b).
6. according to the method described in claim 5, it is characterized in that, containing Na in alkaline solution described in step b)2CO3And/or
NaHCO3。
7. the method according to claim 1, wherein the pre- carbonized samples of step b) are placed in alkaline solution processing is
Stirring no less than 6 hours.
8. the method according to the description of claim 7 is characterized in that the pre- carbonized samples of step b) are placed in alkaline solution processing is
Stirring 6 hours~10 hours.
9. the method according to claim 1, wherein step c) is non-for degreasing sample obtained by step b) to be placed in
In reactive gas atmosphere, system temperature is risen to 600 DEG C~900 DEG C with the heating rate of 1~10 DEG C/min and keeps 0.5~3
After hour is carbonized, it is cooled to room temperature to get the porous carbon materials are arrived.
10. according to claim 1 or method described in 9, which is characterized in that non-active gas described in step c) be selected from nitrogen,
At least one of inert gas.
11. a kind of anode material of lithium-ion battery, which is characterized in that prepared containing method according to any of claims 1 to 10
Obtained porous carbon materials.
12. a kind of sodium-ion battery, which is characterized in that contain the anode material of lithium-ion battery described in claim 11.
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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 |
| CN111204731B (en) * | 2020-01-07 | 2022-05-27 | 大连理工大学 | Preparation method of hard carbon negative electrode material of sodium ion battery |
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