CN110127687A - Artificial graphite and its preparation method and application - Google Patents
Artificial graphite and its preparation method and application Download PDFInfo
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- CN110127687A CN110127687A CN201910440730.6A CN201910440730A CN110127687A CN 110127687 A CN110127687 A CN 110127687A CN 201910440730 A CN201910440730 A CN 201910440730A CN 110127687 A CN110127687 A CN 110127687A
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- 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
- C01B32/20—Graphite
- C01B32/205—Preparation
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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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- 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
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Abstract
The invention discloses a kind of artificial graphites and its preparation method and application, this method comprises: needle-shaped presoma is carried out break process by (1), to obtain D50For 6-15 μm of needle-shaped precursor powder；(2) non-needle-shaped presoma is subjected to break process, to obtain D50For 3-10 μm of non-needle-shaped precursor powder, and the partial size of the non-needle-shaped precursor powder is less than the partial size of the needle-shaped precursor powder；(3) the needle-shaped precursor powder is mixed with the non-needle-shaped precursor powder, binder, to obtain mixed material；(4) mixed material is subjected to graphitization processing, to obtain artificial graphite.The needle-shaped and non-needle-shaped presoma that this method uses partial size different is as raw material, and the partial size of needle-shaped precursor powder is greater than the partial size of non-needle-shaped precursor powder, so that resulting artificial graphite energy density is high, the service life is long and multiplying power is good.
Description
Technical field
The invention belongs to field of lithium, specifically, the present invention relates to artificial graphites and its preparation method and application.
Background technique
Graphite as most important lithium ion battery negative material, be according to type roughly divided into natural graphite, artificial graphite,
Carbonaceous mesophase spherules etc..Wherein artificial graphite with its good electrolyte compatibility and excellent cyclical stability be able to lithium from
It is widely applied in sub- battery.But the artificial graphite mostly capacity of common process manufacture is relatively low, and people generally use items
Anisotropic needle coke promotes the capacity of artificial graphite using following treatment process as presoma: (one) superhigh temperature graphitization；
(2) catalyzed graphitization processing is carried out to artificial graphite presoma using catalyst.By the selection of the above presoma, graphitization
Although processing and etc. after obtained artificial graphite capacity obtained biggish promotion, it is internal since its degree of graphitization is higher
Structural arrangement is more orderly, to lose some advantages of a part of artificial graphite script, such as good charging-discharging structure is steady
Qualitative, higher lithium ion diffusion coefficient etc. causes to fill using the cyclical stability and multiplying power of the lithium ion battery of such material
Discharge performance is affected.
Therefore, the preparation method of existing artificial graphite is further improved.
Summary of the invention
The present invention is directed to solve at least some of the technical problems in related technologies.For this purpose, of the invention
One purpose is to propose a kind of artificial graphite and its preparation method and application.This method needle-shaped and non-needle different using partial size
Shape presoma is as raw material, and the partial size of needle-shaped precursor powder is greater than the partial size of non-needle-shaped precursor powder, so that resulting
Artificial graphite energy density is high, the service life is long and multiplying power is good.
In one aspect of the invention, the invention proposes a kind of method for preparing artificial graphite, realities according to the present invention
Example is applied, this method comprises:
(1) needle-shaped presoma is subjected to break process, to obtain D50For 6-15 μm of needle-shaped precursor powder；
(2) non-needle-shaped presoma is subjected to break process, to obtain D50For 3-10 μm of non-needle-shaped precursor powder, and
The partial size of the non-needle-shaped precursor powder is less than the partial size of the needle-shaped precursor powder；
(3) the needle-shaped precursor powder is mixed with the non-needle-shaped precursor powder, binder, to be mixed
Material；
(4) mixed material is subjected to graphitization processing, to obtain artificial graphite.
The method according to an embodiment of the present invention for preparing artificial graphite, by using needle-shaped and non-needle-shaped presoma as system
The raw material of standby artificial graphite may make the artificial graphite of preparation while have the characteristics that energy density is high, the service life is long and multiplying power is good.
The difference of the partial size of needle-shaped precursor powder and non-needle-shaped precursor powder simultaneously, and the partial size of needle-shaped precursor powder is greater than non-
The partial size of needle-shaped precursor powder is conducive to so that the presoma granule size of the two different structure in mixed process is arranged in pairs or groups
The tap density and compacted density of gained artificial graphite are promoted, and then promotes the energy density of material.Before will be needle-shaped
It drives body powder to mix with non-needle-shaped precursor powder, binder, may make needle-shaped precursor powder and non-needle-shaped precursor powder
Be uniformly mixed, promote the consistency of needle-shaped precursor powder and non-needle-shaped precursor powder everywhere in mixed material, so as into
One step improves the quality of gained artificial graphite.
In addition, the method according to the above embodiment of the present invention for preparing artificial graphite can also have following additional technology
Feature:
In some embodiments of the invention, in step (1), the needle-shaped presoma be selected from petroleum needle coke,
At least one of coal-based needle coke.It can further improve the compaction capacity and capacity of artificial graphite as a result,.
In some embodiments of the invention, in step (2), the non-needle-shaped presoma is fibre structure presoma
And/or mosaic texture presoma.It can further improve the cyclical stability and rate charge-discharge performance of artificial graphite as a result,.
In some embodiments of the invention, in step (2), the fibre structure presoma is selected from fibre structure stone
At least one of oil coke, fibre structure pitch coke.The cyclical stability and multiplying power that can further improve artificial graphite as a result, fill
Discharge performance.
In some embodiments of the invention, in step (2), the mosaic texture presoma is selected from mosaic texture stone
At least one of oil coke, mosaic texture pitch coke.The cyclical stability and multiplying power that can further improve artificial graphite as a result, fill
Discharge performance.
In some embodiments of the invention, in step (3), the needle-shaped precursor powder and the non-needle-shaped forerunner
The mass ratio of body powder is 30-95:5-70, and the quality of the needle-shaped precursor powder is greater than the non-needle-shaped precursor powder
Quality.It can further improve the energy density, cycle life and multiplying power of artificial graphite as a result,.
In some embodiments of the invention, in step (3), the quality of the needle-shaped precursor powder is greater than described non-
The quality of the non-needle-shaped precursor powder of any structure in needle-shaped precursor powder.It can further improve as a result, artificial
Energy density, cycle life and the multiplying power of graphite.
In some embodiments of the invention, in step (3), the binder and the needle-shaped precursor powder and institute
The mass ratio for stating the quality sum of non-needle-shaped precursor powder is 1-30:100.It can further improve the energy of artificial graphite as a result,
Metric density, cycle life and multiplying power.
In some embodiments of the invention, in step (3), the binder be selected from selected from coal tar pitch and petroleum asphalt, in
Between at least one of asphalt phase, phenolic resin, epoxy resin, Petropols.It can further improve the energy of artificial graphite as a result,
Metric density, cycle life and multiplying power.
In some embodiments of the invention, in step (3), the softening point of the binder is 50-300 degrees Celsius.
It can further improve the energy density, cycle life and multiplying power of artificial graphite as a result,.
In some embodiments of the invention, in step (3), the mixing is carried out by the way of heating stirring, and
The revolving speed of the heating stirring is 5-100r/min, and temperature is 250-750 degrees Celsius, time 1-6h.It can further mention as a result,
Energy density, cycle life and the multiplying power of high artificial graphite.
In some embodiments of the invention, in step (4), the temperature of the graphitization processing is taken the photograph for 2400-3000
Family name's degree.It can further improve the energy density, cycle life and multiplying power of artificial graphite as a result,.
In another aspect of the invention, the invention proposes a kind of artificial graphites, according to an embodiment of the invention, described
Artificial graphite is prepared using the above-mentioned method for preparing artificial graphite.As a result, the artificial graphite have energy density it is high,
The fine quality having extended cycle life with good rate capability, relative to the artificial graphite using existing method preparation, the artificial graphite
Not only capacity gets a promotion, and is able to maintain the good charging-discharging structure stability of artificial graphite script, the expansion of higher lithium ion
The advantages that dissipating coefficient.
In an additional aspect of the present invention, the invention proposes a kind of lithium ion batteries, according to an embodiment of the invention, institute
The cathode for stating lithium ion battery is prepared using above-mentioned artificial graphite.It is high by using above-mentioned energy density as a result, follow
The ring service life, the long artificial graphite with good rate capability prepared the cathode of lithium ion battery, can reduce the expansion of cathode, while can mention
Capacity, cyclical stability and the rate charge-discharge performance of high-lithium ion battery.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Above-mentioned and/or additional aspect of the invention and advantage will become from the description of the embodiment in conjunction with the following figures
Obviously and it is readily appreciated that, in which:
Fig. 1 is the method flow schematic diagram according to an embodiment of the invention for preparing artificial graphite.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.
In one aspect of the invention, the invention proposes a kind of method for preparing artificial graphite, realities according to the present invention
Example is applied, with reference to Fig. 1, this method comprises:
S100: needle-shaped presoma is subjected to break process
In the step, needle-shaped presoma is subjected to break process, obtains D50For 6-15 μm of needle-shaped precursor powder.Specifically
, the partial size of needle-shaped precursor powder can be 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm, 15 μm, hair
Bright people's discovery is unfavorable for it and forms size matching with non-needle-shaped presoma and then mention if the partial size of needle-shaped precursor powder is too small
Consolidation effect, while the too small compacting that can also reduce prepared artificial graphite of partial size of needle-shaped precursor powder itself are risen, it is comprehensive
The above two o'clock: the too small artificial graphite compacting that will lead to preparation of the partial size of needle-shaped presoma is relatively low, and pole piece expansion increases, to lead
Causing the artificial graphite energy density of preparation reduces；And the excessive artificial graphite that will lead to preparation of partial size of needle-shaped precursor powder
High rate performance decline is more.A specific embodiment according to the present invention, needle-shaped presoma can for selected from petroleum needle coke,
At least one of coal-based needle coke.Inventors have found that select at least one of petroleum needle coke, coal-based needle coke as
Needle-shaped presoma, prepared artificial graphite capacity is high, compacting is high, and the energy that can greatly promote prepared artificial graphite is close
Degree.S200: non-needle-shaped presoma is subjected to break process
In the step, non-needle-shaped presoma is subjected to break process, obtains D50For 3-10 μm of non-needle-shaped precursor powder,
And the partial size of non-needle-shaped precursor powder is less than the partial size of needle-shaped precursor powder.Specifically, the grain of non-needle-shaped precursor powder
Diameter can be 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm.Inventors have found that the partial size of needle-shaped precursor powder is greater than
The partial size of non-needle-shaped precursor powder can make the two presoma granule size of different structure in subsequent mixed process take
Match, is conducive to the tap density and compacted density that promote gained artificial graphite, and then promote the energy density of material.Further
, if not the partial size of needle-shaped precursor powder is too small, then it is easy to reunite, cannot be formed with needle-shaped precursor powder, binder
One mixture；If not the partial size of needle-shaped precursor powder is excessive, then be unfavorable for its formed with needle-shaped presoma size matching into
And the effect of compacting is promoted, while the partial size of non-needle-shaped precursor powder crosses the high rate performance of the prepared artificial graphite of conference reduction
And cycle performance.A specific embodiment according to the present invention, non-needle-shaped presoma can be fibre structure presoma and/or edge
Embedding structured forerunner.Inventors have found that artificial graphite isotropic structure prepared by above-mentioned non-needle-shaped presoma is preferable, Li+
Intercalation/deintercalation is relatively easy, and rate charge-discharge performance and circulation performance are relatively preferable.Fibre structure presoma can be choosing
From at least one of fibre structure petroleum coke, fibre structure pitch coke.Inventors have found that above-mentioned fibre structure presoma can be into
The rate charge-discharge performance and circulation performance of one step raising artificial graphite.Mosaic texture presoma can for selected from inlay knot
At least one of structure petroleum coke, mosaic texture pitch coke.Inventors have found that above-mentioned mosaic texture presoma can further improve
The rate charge-discharge performance and circulation performance of artificial graphite, and artificial graphite multiplying power charge and discharge prepared by embedding structured forerunner
Electrical property and circulation performance are better than artificial graphite prepared by fibre structure presoma.
It should be noted that the sequencing of step S100 and step S200 are not limited because of serial number in the application, it is real
Border can first prepare non-needle-shaped precursor powder, can also first prepare needle-shaped precursor powder, or both respectively while prepare
It is all right.
S300: needle-shaped precursor powder is mixed with non-needle-shaped precursor powder, binder
In the step, needle-shaped precursor powder is mixed with non-needle-shaped precursor powder, binder, obtains mixed material.
Inventors have found that may make the artificial of preparation as the raw material for preparing artificial graphite by using needle-shaped and non-needle-shaped presoma
Graphite has the characteristics that energy density is high, the service life is long and multiplying power is good simultaneously.Simultaneously needle-shaped precursor powder partial size with it is non-needle-shaped
The difference of precursor powder, and the partial size of needle-shaped precursor powder is greater than the partial size of non-needle-shaped precursor powder, so that the two exists
The presoma granule size collocation of different structure, is conducive to the tap density and compacting that promote gained artificial graphite in mixed process
Density, and then promote the energy density of material.Additionally by by needle-shaped precursor powder and non-needle-shaped precursor powder, binder
Mixing, may make needle-shaped precursor powder to be uniformly mixed with non-needle-shaped precursor powder, before needle-shaped everywhere in promotion mixed material
The consistency for driving body powder and non-needle-shaped precursor powder, to can further improve the quality that income earner makes graphite.
According to one embodiment of present invention, the mass ratio of needle-shaped precursor powder and non-needle-shaped precursor powder can be
30-95:5-70, such as can be (30/35/40/45/50/55/60/65/70/75/80/85/90/95): (5/10/15/20/
25/30/35/40/45/50/55/60/65/70), and the quality of needle-shaped precursor powder be greater than non-needle-shaped precursor powder matter
Amount.Inventors have found that the mass ratio of needle-shaped precursor powder and non-needle-shaped precursor powder is excessively high, prepared artificial stone can be reduced
The high rate performance of ink；And the mass ratio of needle-shaped precursor powder and non-needle-shaped precursor powder is too low, then can reduce prepared people
Make the energy density of graphite.The quality of a specific embodiment according to the present invention, needle-shaped precursor powder can be greater than non-needle
The quality of the non-needle-shaped precursor powder of any structure in shape precursor powder.Inventors have found that needle-shaped precursor powder
It is good to be orientated consistency, the structure more high-sequential after graphitization processing, thus its capacity and compacted density are higher.Before needle-shaped
The quality for driving body powder is greater than the quality of the non-needle-shaped precursor powder of any structure in non-needle-shaped precursor powder, Neng Gouxian
Write the energy density for promoting prepared artificial graphite.According to one embodiment of present invention, binder and needle-shaped precursor
The mass ratio of the quality sum of last and non-needle-shaped precursor powder can be 1-30:100, such as can be (1/5/10/15/20/
25/30): 100.Inventors have found that the accounting of binder is too low, then granulation outcome is bad, and prepared artificial graphite items are same
Property performance is bad, can be unfavorable for the promotion of the high rate performance of material in this way；And the accounting of binder is excessively high, then can reduce prepared
Artificial graphite energy density.A specific embodiment according to the present invention, binder can be for selected from coal tar pitch, petroleum drip
At least one of blueness, mesophase pitch, phenolic resin, epoxy resin, Petropols.Inventors have found that the bonding of pitch class
Structure of the agent after graphitization is relatively orderly, uses the first charge discharge efficiency and capacity of artificial graphite prepared by pitch class binder
It is relatively high；And the binder of resinae degree of disorder after graphitization is high, uses artificial stone prepared by bonded adhesive
Black cryogenic property and high rate performance are relatively preferable.Another specific embodiment according to the present invention, the softening point of binder can be with
It is 50-300 degrees Celsius, such as can is 50 degrees Celsius, 75 degrees Celsius, 100 degrees Celsius, 125 degrees Celsius, 150 degrees Celsius, 175
Degree Celsius, 200 degrees Celsius, 225 degrees Celsius, 250 degrees Celsius, 275 degrees Celsius, 300 degrees Celsius.Inventors have found that binder
Softening point is too low, then is unfavorable for the holding of mixture particle pattern after being granulated；The softening point of binder is excessively high, then Hybrid Heating
When mixed material poor fluidity, be unfavorable for the graphitization processing of mixed material.
Still another embodiment in accordance with the present invention, mixing can be carried out by the way of heating stirring, and heating stirring
Revolving speed can be 5-100r/min, such as can be 5r/min, 10r/min, 15r/min, 20r/min, 25r/min, 30r/
min、35r/min、40r/min、45r/min、50r/min、55r/min、60r/min、65r/min、70r/min、75r/min、
80r/min, 85r/min, 90r/min, 95r/min, 100r/min, temperature can be 250-750 degrees Celsius, such as can be
250 degrees Celsius, 300 degrees Celsius, 350 degrees Celsius, 400 degrees Celsius, 450 degrees Celsius, 500 degrees Celsius, 550 degrees Celsius, it is 600 Celsius
Degree, 650 degrees Celsius, 700 degrees Celsius, time can be 1-6h, such as can be 1h, 2h, 3h, 4h, 5h, 6h.Inventors have found that
If temperature is too low when heating stirring, binder is not fully developed flow regime, is unfavorable for binder in precursor powder table
Complete cladding on face, mixing speed is too low be equally unfavorable for binder and precursor powder, different precursor powders it is uniform
Mixing；And temperature when heating stirring is excessively high, mixing time is too long causes greatly to waste to efficiency and equipment cost.
S400: mixed material is subjected to graphitization processing
In the step, mixed material is subjected to graphitization processing, to obtain artificial graphite.Inventors have found that in high temperature
During processing, the structure of mixed material gradually changes to the graphite-structure of more ordering, finally obtains with height stone
The artificial graphite material of inkization.
According to one embodiment of present invention, the temperature of graphitization processing can be 2400-3000 degrees Celsius, such as can be with
For 2400 degrees Celsius, 2500 degrees Celsius, 2600 degrees Celsius, 2700 degrees Celsius, 2800 degrees Celsius, 2900 degrees Celsius, it is 3000 Celsius
Degree.Inventors have found that the temperature of graphitization processing is too low, the degree of graphitization of mixed material is low, is unfavorable for the artificial stone of preparation
The promotion of the capacity and compaction capacity of ink；The temperature of graphitization processing is excessively high, then can reduce the multiplying power of prepared artificial graphite
And cycle performance.
The method according to an embodiment of the present invention for preparing artificial graphite, by using needle-shaped and non-needle-shaped presoma as system
The raw material of standby artificial graphite may make the artificial graphite of preparation while have the characteristics that energy density is high, the service life is long and multiplying power is good.
The difference of the partial size of needle-shaped precursor powder and non-needle-shaped precursor powder simultaneously, and the partial size of needle-shaped precursor powder is greater than non-
The partial size of needle-shaped precursor powder is conducive to so that the presoma granule size of the two different structure in mixed process is arranged in pairs or groups
The tap density and compacted density of gained artificial graphite are promoted, and then promotes the energy density of material.Before will be needle-shaped
It drives body powder to mix with non-needle-shaped precursor powder, binder, may make needle-shaped precursor powder and non-needle-shaped precursor powder
Be uniformly mixed, promote the consistency of needle-shaped precursor powder and non-needle-shaped precursor powder everywhere in mixed material, so as into
One step improves the quality of gained artificial graphite.
In another aspect of the invention, the invention proposes a kind of artificial graphites, according to an embodiment of the invention, the people
Making graphite is prepared using the above-mentioned method for preparing artificial graphite.The artificial graphite has energy density height, follows as a result,
The ring service life long fine quality with good rate capability, relative to the artificial graphite using existing method preparation, the artificial graphite is not
Only capacity gets a promotion, and is able to maintain the good charging-discharging structure stability of artificial graphite script, the diffusion of higher lithium ion
The advantages that coefficient.It should be noted that the feature and advantage of the above-mentioned method for preparing artificial graphite are equally applicable to the artificial stone
Ink repeats no more this.
In an additional aspect of the present invention, the invention proposes a kind of lithium ion batteries, according to an embodiment of the invention, should
The cathode of lithium ion battery is prepared using above-mentioned artificial graphite.High by using above-mentioned energy density as a result, circulation
Service life, the long artificial graphite with good rate capability prepared the cathode of lithium ion battery, can reduce the expansion of cathode, can be improved simultaneously
Capacity, cyclical stability and the rate charge-discharge performance of lithium ion battery.It should be noted that the feature of above-mentioned artificial graphite and
Advantage is equally applicable to the negative electrode of lithium ion battery, repeats no more to this.
Below with reference to specific embodiment, present invention is described, it should be noted that these embodiments are only to describe
Property, without limiting the invention in any way.
Embodiment 1
Needle-shaped presoma petroleum needle coke is subjected to break process, obtains D50For 6 μm of needle-shaped precursor powder；
Non- acicular petroleum coke presoma with fibre structure is subjected to break process, obtains D50For 3 μm it is non-it is needle-shaped before
Drive body powder；
Above-mentioned needle-shaped precursor powder and above-mentioned non-needle-shaped precursor powder, coal pitch of agglomerant and asphalt are heated
It is stirred, obtains mixed material.Wherein, above-mentioned needle-shaped precursor powder is with above-mentioned non-needle-shaped precursor powder mass ratio
30:5；The mass ratio of the quality sum of binder and above-mentioned needle-shaped precursor powder and non-needle-shaped precursor powder is 1:100；Coal
The softening point of pitch and asphalt is 180 degrees Celsius, and the mass ratio of coal tar pitch and asphalt is 1:1；Heating stirring
Revolving speed is 5r/min, and temperature is 250 degrees Celsius, time 6h；
Said mixture material is subjected to graphitization processing under 2400 degrees Celsius, obtains artificial graphite.
Embodiment 2
Needle-shaped presoma coal-based needle coke is subjected to break process, obtains D50For 10 μm of needle-shaped precursor powder；
There to be the non-needle-shaped pitch coke presoma of mosaic texture to carry out break process, and obtain D50For 6 μm of non-needle-shaped forerunner
Body powder；
Above-mentioned needle-shaped precursor powder and above-mentioned non-needle-shaped precursor powder, binder mesophase pitch heating stirring are mixed
It closes, obtains mixed material.Wherein, above-mentioned needle-shaped precursor powder and above-mentioned non-needle-shaped precursor powder mass ratio are 60:35；It is viscous
The mass ratio for tying the quality sum of agent and above-mentioned needle-shaped precursor powder and non-needle-shaped precursor powder is 15:100；Interphase drip
Green softening point is 295 degrees Celsius；The revolving speed of heating stirring is 50r/min, and temperature is 500 degrees Celsius, time 3h；
Said mixture material is subjected to graphitization processing under 2700 degrees Celsius, obtains artificial graphite.
Embodiment 3
Needle-shaped presoma petroleum needle coke is subjected to break process, obtains D50For 15 μm of needle-shaped precursor powder；
By with fibre structure non-acicular petroleum coke presoma and have the non-needle-shaped pitch coke presoma of mosaic texture into
Row break process, obtains D50For 10 μm of non-needle-shaped precursor powder；
Above-mentioned needle-shaped precursor powder and above-mentioned non-needle-shaped precursor powder, adhesive phenolic resin heating stirring are mixed
It closes, obtains mixed material.Wherein, above-mentioned needle-shaped precursor powder and above-mentioned non-needle-shaped precursor powder mass ratio are 95:70；It is viscous
The mass ratio for tying the quality sum of agent and above-mentioned needle-shaped precursor powder and non-needle-shaped precursor powder is 30:100；Phenolic resin
Softening point be 90 degrees Celsius, the revolving speed of heating stirring is 100r/min, and temperature is 750 degrees Celsius, time 1h；
Said mixture material is subjected to graphitization processing under 3000 degrees Celsius, obtains artificial graphite.
Embodiment 4
Needle-shaped presoma petroleum needle coke and coal-based needle coke are subjected to break process, obtain D50For before 8 μm needle-shaped
The mass ratio of drive body powder, petroleum needle coke and coal-based needle coke is 1:1；
The non-needle-shaped presoma of mosaic texture is subjected to break process, obtains D50For 5 μm of non-needle-shaped precursor powder；
Above-mentioned needle-shaped precursor powder and above-mentioned non-needle-shaped precursor powder, epoxy resin of binder heating stirring are mixed
It closes, obtains mixed material.Wherein, above-mentioned needle-shaped precursor powder and above-mentioned non-needle-shaped precursor powder mass ratio are 50:30；It is viscous
The mass ratio for tying the quality sum of agent epoxy resin and above-mentioned needle-shaped precursor powder and non-needle-shaped precursor powder is 20:100；
The softening point of epoxy resin is 83 degrees Celsius；The revolving speed of heating stirring is 30r/min, and temperature is 300 degrees Celsius, time 4h；
Said mixture material is subjected to graphitization processing under 2600 degrees Celsius, obtains artificial graphite.
Embodiment 5
Needle-shaped presoma petroleum needle coke is subjected to break process, obtains D50For 12 μm of needle-shaped precursor powder；
The non-needle-shaped presoma of fibre structure is subjected to break process, obtains D50For 8 μm of non-needle-shaped precursor powder；
Above-mentioned needle-shaped precursor powder and above-mentioned non-needle-shaped precursor powder, binder Petropols heating stirring are mixed
It closes, obtains mixed material.Wherein, above-mentioned needle-shaped precursor powder and above-mentioned non-needle-shaped precursor powder mass ratio are 40:10；It is viscous
The mass ratio for tying the quality sum of agent Petropols and above-mentioned needle-shaped precursor powder and non-needle-shaped precursor powder is 28:100；
The softening point of Petropols is 150 degrees Celsius；The revolving speed of heating stirring is 70r/min, and temperature is 550 degrees Celsius, time 2h；
Said mixture material is subjected to graphitization processing under 2500 degrees Celsius, obtains artificial graphite.
It the use of cobalt acid lithium is positive electrode, embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 are prepared
Artificial graphite be negative electrode material, carries out maximum compacting respectively to negative electrode tab, be respectively made the polymer lithiums of 554065 models from
Sub- battery.The 100%SOC pole piece expansion rate of the preparation-obtained lithium ion battery of the resulting artificial graphite of embodiment 1-5 is held
Amount, cycle performance, high rate performance are as shown in table 1.As shown in Table 1, by the compacting of the preparation-obtained artificial graphite of embodiment 1-5
Density is higher, and gained pole piece expansion rate is lower, and is protected using the battery core capacity of its lithium ion battery being prepared, circulation volume
Holdup and multiplying power are higher.
The performance data of the compacting situation of artificial graphite preparation negative electrode tab and respective battery obtained by 1 embodiment 1-5 of table
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (10)
1. a kind of method for preparing artificial graphite characterized by comprising
(1) needle-shaped presoma is subjected to break process, to obtain D50For 6-15 μm of needle-shaped precursor powder；
(2) non-needle-shaped presoma is subjected to break process, to obtain D50For 3-10 μm of non-needle-shaped precursor powder, and it is described
The partial size of non-needle-shaped precursor powder is less than the partial size of the needle-shaped precursor powder；
(3) the needle-shaped precursor powder is mixed with the non-needle-shaped precursor powder, binder, to obtain mixture
Material；
(4) mixed material is subjected to graphitization processing, to obtain artificial graphite.
2. the method according to claim 1, wherein the needle-shaped presoma is selected from petroleum in step (1)
It is at least one of needle coke, coal-based needle coke.
3. the method according to claim 1, wherein the non-needle-shaped presoma is fiber knot in step (2)
Structure presoma and/or mosaic texture presoma；
Optional, in step (2), the fibre structure presoma is selected from fibre structure petroleum coke, fibre structure pitch coke
At least one of；
Optional, in step (2), the mosaic texture presoma is selected from mosaic texture petroleum coke, mosaic texture pitch coke
At least one of.
4. the method according to claim 1, wherein in step (3), the needle-shaped precursor powder with it is described
The mass ratio of non-needle-shaped precursor powder is 30-95:5-70, and the quality of the needle-shaped precursor powder is greater than described non-needle-shaped
The quality of precursor powder.
5. according to the method described in claim 3, it is characterized in that, in step (3), the quality of the needle-shaped precursor powder
Greater than the quality of the non-needle-shaped precursor powder of any structure in the non-needle-shaped precursor powder.
6. the method according to claim 1, wherein in step (3), the binder and the needle-shaped forerunner
The mass ratio of the quality sum of body powder and the non-needle-shaped precursor powder is 1-30:100；
Optional, in step (3), the binder is selected from selected from coal tar pitch and petroleum asphalt, mesophase pitch, phenolic resin, ring
At least one of oxygen resin, Petropols；
Optional, in step (3), the softening point of the binder is 50-300 degrees Celsius.
7. the method according to claim 1, wherein the mixing uses the side of heating stirring in step (3)
Formula carries out, and the revolving speed of the heating stirring is 5-100r/min, and temperature is 250-750 degrees Celsius, time 1-6h.
8. the method according to claim 1, wherein in step (4), the temperature of the graphitization processing is
2400-3000 degrees Celsius.
9. a kind of artificial graphite, which is characterized in that the artificial graphite is using method of any of claims 1-8
It is prepared.
10. a kind of lithium ion battery, which is characterized in that the cathode of the lithium ion battery is using people as claimed in claim 9
Make what graphite was prepared.
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| CN112133894A (en) * | 2020-09-03 | 2020-12-25 | 深圳石墨烯创新中心有限公司 | Negative electrode material for lithium battery and preparation method of material |
| CN115448305A (en) * | 2022-09-19 | 2022-12-09 | 惠州锂威新能源科技有限公司 | Graphite matrix and preparation method thereof, and quick-charging graphite and preparation method thereof |
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