CN108598478A - Modified graphite preparation method and modified graphite - Google Patents
Modified graphite preparation method and modified graphite Download PDFInfo
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- CN108598478A CN108598478A CN201810382075.9A CN201810382075A CN108598478A CN 108598478 A CN108598478 A CN 108598478A CN 201810382075 A CN201810382075 A CN 201810382075A CN 108598478 A CN108598478 A CN 108598478A
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- modified graphite
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- mixed slurry
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- intermediate product
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- 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 modified graphite preparation method and modified graphites, are related to cell manufacturing techniques field.The present invention provides a kind of modified graphite preparation method, is used to prepare modified graphite, modified graphite preparation method includes:Natural spherical plumbago, cladding carbon source and organic solvent are mixed, the first mixed slurry is obtained.First mixed slurry is put into wet grinding mill, and the first mixed slurry is stirred, obtains the second mixed slurry.Second mixed slurry is spray-dried, and obtains the first product.Carbonization treatment is carried out to the first product, obtains the second product.Sieving is ground to the second product, obtains modified graphite.A kind of modified graphite is made by above-mentioned modified graphite preparation method.Modified graphite preparation method provided by the invention and modified graphite can improve the stability, specific capacity and cycle performance of modified graphite.
Description
Technical field
The present invention relates to cell manufacturing techniques fields, in particular to modified graphite preparation method and modified graphite.
Background technology
In actual life, the promotion dynamics for new energy is increasing, wherein for recycling the use of electric energy
It is more and more common, wherein being also more and more common for the use of the battery of cycle charging.
For existing cycle charging battery, natural graphite is mostly used greatly, but the specific capacity of natural graphite is smaller, and
After multiple charge-discharge cycle, the reserve of electricity of rechargeable battery declines very fast, and the service life of battery is caused to decline, waste largely at
This.
Invention content
The purpose of the present invention is to provide a kind of modified graphite preparation method, the stability of the modified graphite prepared, ratio
Capacity and cycle performance can be improved.
Another object of the present invention is to provide a kind of modified graphite, stability, specific capacity and cycle performance obtain
It improves.
The present invention provides a kind of technical solution:
A kind of modified graphite preparation method, is used to prepare modified graphite, and the modified graphite preparation method includes:
Natural spherical plumbago, cladding carbon source and organic solvent are mixed, the first mixed slurry is obtained.
First mixed slurry is put into wet grinding mill, and first mixed slurry is stirred, is obtained
To the second mixed slurry.
Second mixed slurry is spray-dried, and obtains the first product.
Carbonization treatment is carried out to first product, obtains the second product.
Sieving is ground to second product, obtains modified graphite.
Further, described that first mixed slurry is put into wet grinding mill, and to first mixing slurry
Material is stirred, and is obtained the second mixed slurry step and is included:First mixed slurry is being put into the wet grinding mill, and
The first mixed slurry is stirred under normal temperature environment, obtains the second mixed slurry.
Further, 3h~15h is stirred to first mixed slurry.
Further, the speed that first mixed slurry is stirred in control is 1600r/min~3200r/min.
Further, it is 2 μm~5 μm to control the graphite grain size in second mixed slurry.
Further, described to carry out carbonization treatment to first product, obtaining the second product step includes:
Sieving processing is carried out to first product, obtains the first intermediate product.
Level-one carbonization treatment is carried out to first intermediate product, obtains the second intermediate product.
Sieving processing is carried out to second intermediate product, obtains third intermediate product.
Two level carbonization treatment is carried out to the third intermediate product, obtains the second product.
Further, described to first intermediate product progress and carbonization treatment, obtain the second intermediate product step
Including:First intermediate product is put into tube furnace, is 400 DEG C~600 DEG C by the temperature control in the tube furnace, obtains
To the second intermediate product.
Further, described that two level carbonization treatment is carried out to the third intermediate product, obtain the second product step packet
It includes:Third intermediate product is put into tube furnace, and is 800 DEG C~1000 DEG C by the temperature control in tube furnace, obtains the
Two products.
Further, the time control for calcining second intermediate product is 3h~10h.
A kind of modified graphite is made of modified graphite preparation method.The modified graphite preparation method includes:
Natural spherical plumbago, cladding carbon source and organic solvent are mixed, the first mixed slurry is obtained.
First mixed slurry is put into wet grinding mill, and first mixed slurry is stirred, is obtained
To the second mixed slurry.
Second mixed slurry is spray-dried, and obtains the first product.
Carbonization treatment is carried out to first product, obtains the second product.
Sieving is ground to second product, obtains modified graphite.
Compared with prior art, the advantageous effect of modified graphite preparation method provided by the invention is:
Modified graphite preparation method provided by the invention is by mixing natural graphite, cladding carbon source and organic solvent
After the modified graphite that carries out wet grinding, and obtained by the method for spray drying and carbonization, calcining, sieving and grinding,
Stability, specific capacity and the cycle performance of the modified graphite get a promotion.
Compared with prior art, the advantageous effect of modified graphite provided by the invention is:
Modified graphite provided by the invention is made up of above-mentioned modified graphite preparation method, the stability of modified graphite,
Specific capacity and cycle performance get a promotion.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described.It should be appreciated that the following drawings illustrates only certain embodiments of the present invention, therefore it is not construed as pair
The restriction of range.It for those of ordinary skill in the art, without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the flow diagram for the modified graphite preparation method that the first embodiment of the present invention provides;
Fig. 2 is the flow diagram for the step S104 that the first embodiment of the present invention provides;
Fig. 3 is the flow diagram for the step S1042 that the first embodiment of the present invention provides;
Fig. 4 is the flow diagram for the step S1044 that the first embodiment of the present invention provides;
Fig. 5 is graphite modified front and back for charging and discharging curve comparison diagram for the first time;
Fig. 6 is graphite modified front and back material circulation comparison diagram.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described.Obviously, described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.The present invention being usually described and illustrated herein in the accompanying drawings is implemented
The component of example can be arranged and be designed with a variety of different configurations.
Therefore, below the detailed description of the embodiment of the present invention to providing in the accompanying drawings be not intended to limit it is claimed
The scope of the present invention, but be merely representative of the present invention selected embodiment.Based on the embodiments of the present invention, this field is common
The every other embodiment that technical staff is obtained without creative efforts belongs to the model that the present invention protects
It encloses.
It should be noted that:Similar label and letter indicate similar terms in following attached drawing, therefore, once a certain Xiang Yi
It is defined, then it further need not be defined and explained in subsequent attached drawing in a attached drawing.
In the description of the present invention, it is to be understood that, the instructions such as term "upper", "lower", "inner", "outside", "left", "right"
Orientation or positional relationship be based on the orientation or positional relationship shown in the drawings or the invention product using when usually put
Orientation or positional relationship or the orientation or positional relationship that usually understands of those skilled in the art, be merely for convenience of retouching
It states the present invention and simplifies description, do not indicate or imply the indicated equipment or element must have a particular orientation, with specific
Azimuth configuration and operation, therefore be not considered as limiting the invention.
In addition, term " first ", " second " etc. are only used for distinguishing description, it is not understood to indicate or imply relatively important
Property.
In the description of the present invention, it is also necessary to which explanation is unless specifically defined or limited otherwise, " setting ", " even
Connect " etc. terms shall be understood in a broad sense, for example, " connection " may be a fixed connection, may be a detachable connection, or integrally connect
It connects;It can be mechanical connection, can also be electrical connection;Can be directly connected to, can also be indirectly connected with by intermediary, it can
To be the connection inside two elements.For the ordinary skill in the art, can understand as the case may be above-mentioned
The concrete meaning of term in the present invention.
Below in conjunction with the accompanying drawings, the specific implementation mode of the present invention is described in detail.
First embodiment
Referring to Fig. 1, providing a kind of modified graphite preparation method in the present embodiment, it is used to prepare modified graphite.It is logical
Crossing stability, specific capacity and the cycle performance of the modified graphite of modified graphite preparation method preparation can get a promotion.
Wherein, the step of modified graphite preparation method is as follows:
S101, natural spherical plumbago, cladding carbon source and organic solvent are mixed, obtains the first mixed slurry.
Wherein, in the present embodiment, phenolic resin or pitch may be used in cladding carbon source.Second may be used in organic solvent
Alcohol, carbon disulfide or kerosene.It should be noted that when coating carbon source using phenolic resin, organic solvent needs to use second
Alcohol;When coating carbon source using pitch, organic solvent uses carbon disulfide or kerosene.Wherein, it can be dissolved by organic solvent
Coat carbon source so that cladding carbon source can adequately be spread, and ensure the carry out coating function that cladding carbon source is stablized.
In addition, in the present embodiment, the amount for taking natural spherical plumbago is 85g~106g, the amount for coating carbon source be 2g~
15g.It should be appreciated that in other embodiments, the amount of natural spherical plumbago and the amount of cladding carbon source can be selected according to actual demand
It takes.
S102, the first mixed slurry is put into wet grinding mill, and the first mixed slurry is stirred, obtain
Two mixed slurries.
Wherein, step S102 includes:
First mixed slurry is put into wet grinding mill, and the first mixed slurry is stirred under normal temperature environment
It mixes, obtains the second mixed slurry.
It should be noted that in the present embodiment, wet grinding mill is using explosion-proof wet grinding mill.
Further, in the present embodiment, 3h~15h is stirred to the first mixed slurry.So that the first mixing slurry
Each raw material in material can be uniformly mixed, and ensure the stability of modified graphite obtained.
In addition, the speed of control the first mixed slurry of stirring is 1600r/min~3200r/min.
Also, it is 2 μm~5 μm to control the graphite grain size in the second mixed slurry.
S103, the second mixed slurry is spray-dried, and obtains the first product.
Wherein, step S103 includes:
Second mixed slurry is filled in the form of spraying in closed spray-drying installation, with by closed environment
The middle drying for carrying out the second mixed slurry so that sundries is few in the first product being dried to obtain.And it is sprayed by solvent type
It is dry that common water-based spray drying is replaced to solve the problems, such as that carbon source selection is limited.It can be chosen using solvent type spray drying
Carbon source range expand, while closer to industrial process.
S104, carbonization treatment is carried out to the first product, obtains the second product.
Such as Fig. 2, wherein step S104 includes:
S1041, sieving processing is carried out to the first product, obtains the first intermediate product.
Sieving processing is carried out to the first product, the first product is purified, can make the modified graphite finally obtained
Quality higher avoids too many impurity from being entrained in modified graphite, ensures the stability, specific capacity and cycle performance of modified graphite
It can preferably be promoted.
It should be noted that in the present embodiment, being carried out at sieving using the first product of sieving tool pair of 400 mesh
Reason.
S1042, level-one carbonization treatment is carried out to the first intermediate product, obtains the second intermediate product.
As Fig. 3, step S1042 include:
S10421, the first intermediate product is put into tube furnace.
Wherein, while the first intermediate product is put into tube furnace, protective gas is filled with into tube furnace, wherein
In the present embodiment, protective gas uses Ar, it should be understood that in other embodiments, can also use other inertia such as nitrogen
Gas is as protective gas.
S10422, by tube furnace temperature control be 400 DEG C~600 DEG C, obtain the second intermediate product.
Wherein, the first intermediate product is sintered in tube furnace, is tentatively carbonized to the first intermediate product.That is,
It is 400 DEG C~600 DEG C by the temperature control in tube furnace, and keeps the temperature the first preset time, so that in first in tube furnace
Between product can adequately be carbonized.Operator can in the light of actual conditions control the length of the first preset time, in control first
Between product carbonizing degree.
S1043 carries out sieving processing to the second intermediate product, obtains third intermediate product.
Wherein, the second intermediate product is taken out from tube furnace, and be sieved to the second intermediate product, selected in second
Between graphite grain size is 2 μm~5 μm in product part, which is then third intermediate product.
S1044, two level carbonization treatment is carried out to third intermediate product, obtains the second product.
Such as Fig. 4, wherein step S1044 includes:
S10441, third intermediate product is put into tube furnace.
It should be noted that while the second product is put into tube furnace, protective gas is filled with into tube furnace,
Protective gas uses Ar protective gas.In other are embodiment, the inert gases such as nitrogen can also be used as protective gas.
S10442, by tube furnace temperature control be 800 DEG C~1000 DEG C, obtain the second product.
Wherein, it is 800 DEG C~1000 DEG C by the temperature control in tube furnace, and at the heat preservation of the second preset time of progress
Reason.Second preset time can be configured according to actual demand.
Further, in the present embodiment, the time control of calcining third intermediate product is 3h~10h.That is, in this reality
It applies in example, the temperature in tube furnace is controlled when between 800 DEG C~1000 DEG C, the temperature in tube furnace is subjected to isothermal holding
3h~10h is to get to the second product.
S105, sieving is ground to the second product, obtains modified graphite.
Wherein, the sieving processing of the second product is carried out using the sieving tool of 400 mesh.
The modified graphite preparation method provided in the present embodiment is by carrying out natural graphite, cladding carbon source and organic solvent
Wet grinding, and the modification stone obtained by the method for spray drying and carbonization, calcining, sieving and grinding are carried out after mixing
Ink, stability, specific capacity and the cycle performance of the modified graphite get a promotion.
Second embodiment
A kind of modified graphite is provided in the present embodiment, stability, specific capacity and cycle performance are improved.
Wherein, the modified graphite provided in the present embodiment passes through the modified graphite preparation method system that is provided in first embodiment
.
Please refer to Fig. 5 and Fig. 6, wherein the curve that A is referred in Fig. 5 represents before modified that natural spherical plumbago is for the first time
Charge graph, the curve that B is referred to represent the initial charge curve graph of modified natural spherical plumbago.In figure 6, C curve refers to
Generation be natural spherical plumbago cycle-index and reversible capacity relationship scatter plot, D curves refer to is modified graphite cycle time
The relationship scatter plot of number and reversible capacity.It can be found that after 50 cycles, the charge specific capacity of the modified graphite of preparation is obviously high
In natural spherical plumbago.And it can be found that the reversible capacity of modified material is significantly increased, the specific volume under high magnification
Amount display is better than natural spherical plumbago, and decaying specific capacity will be well below natural spherical plumbago every time.
3rd embodiment
A kind of graphite button cell is provided in the present embodiment, which employs the modified graphites provided in second embodiment.
In the present embodiment, graphite button cell includes lithium piece, modified graphite, conductive agent, diaphragm and electrolyte.Wherein lithium
Anode of the piece as graphite button cell, cathode of the modified graphite as graphite button cell.And, wherein diaphragm uses
Celgard2400, conductive agent use super-p, electrolyte to select the LiPF6 conductive salts and DMC of 1mol/L:DEC:EC
(wt%)=1:1:1 solvent.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of modified graphite preparation method, is used to prepare modified graphite, which is characterized in that the modified graphite preparation method packet
It includes:
Natural spherical plumbago, cladding carbon source and organic solvent are mixed, the first mixed slurry is obtained;
First mixed slurry is put into wet grinding mill, and first mixed slurry is stirred, obtains
Two mixed slurries;
Second mixed slurry is spray-dried, and obtains the first product;
Carbonization treatment is carried out to first product, obtains the second product;
Sieving is ground to second product, obtains modified graphite.
2. modified graphite preparation method according to claim 1, which is characterized in that described to put first mixed slurry
Enter into wet grinding mill, and first mixed slurry is stirred, obtaining the second mixed slurry step includes:By first
Mixed slurry is being put into the wet grinding mill, and is stirred to the first mixed slurry under normal temperature environment, obtains
Two mixed slurries.
3. modified graphite preparation method according to claim 2, which is characterized in that stir first mixed slurry
Mix 3h~15h.
4. modified graphite preparation method according to claim 2, which is characterized in that first mixed slurry is stirred in control
Speed be 1600r/min~3200r/min.
5. modified graphite preparation method according to claim 2, which is characterized in that in control second mixed slurry
Graphite grain size is 2 μm~5 μm.
6. modified graphite preparation method according to claim 1, which is characterized in that described to be carried out to first product
Carbonization treatment, obtaining the second product step includes:
Sieving processing is carried out to first product, obtains the first intermediate product;
Level-one carbonization treatment is carried out to first intermediate product, obtains the second intermediate product;
Sieving processing is carried out to second intermediate product, obtains third intermediate product
Two level carbonization treatment is carried out to the third intermediate product, obtains the second product.
7. modified graphite preparation method according to claim 6, which is characterized in that it is described to first intermediate product into
Row level-one carbonization treatment, obtaining the second intermediate product step includes:First intermediate product is put into tube furnace, it will be described
Temperature control in tube furnace is 400 DEG C~600 DEG C, obtains the second intermediate product.
8. modified graphite preparation method according to claim 6, which is characterized in that it is described to the third intermediate product into
Row two level carbonization treatment, obtaining the second product step includes:Third intermediate product is put into tube furnace, and by tube furnace
In temperature control be 800 DEG C~1000 DEG C, obtain the second product.
9. modified graphite preparation method according to claim 8, which is characterized in that calcine the third intermediate product when
Between control be 3h~10h.
10. a kind of modified graphite, which is characterized in that by the modified graphite preparation method described in any one of claim 1-9
It is made.
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Cited By (2)
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CN111244431A (en) * | 2020-03-20 | 2020-06-05 | 金妍 | Preparation method of lithium ion battery cathode slurry |
CN113372974A (en) * | 2021-06-16 | 2021-09-10 | 扬州市职业大学(扬州市广播电视大学) | Green and environment-friendly new energy material and preparation method thereof |
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