CN114512652A - Process for reducing specific surface area of graphite negative electrode material of lithium battery - Google Patents
Process for reducing specific surface area of graphite negative electrode material of lithium battery Download PDFInfo
- Publication number
- CN114512652A CN114512652A CN202210159883.5A CN202210159883A CN114512652A CN 114512652 A CN114512652 A CN 114512652A CN 202210159883 A CN202210159883 A CN 202210159883A CN 114512652 A CN114512652 A CN 114512652A
- Authority
- CN
- China
- Prior art keywords
- graphite
- crushing
- asphalt
- particles
- spherical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 183
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 171
- 239000010439 graphite Substances 0.000 title claims abstract description 171
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 21
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 81
- 239000010426 asphalt Substances 0.000 claims abstract description 68
- 238000005516 engineering process Methods 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 19
- 229910021382 natural graphite Inorganic materials 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000010406 cathode material Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 229910021385 hard carbon Inorganic materials 0.000 claims abstract description 9
- 238000012216 screening Methods 0.000 claims abstract description 6
- 238000012545 processing Methods 0.000 claims description 30
- 239000002994 raw material Substances 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 239000013078 crystal Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 238000010000 carbonizing Methods 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 238000004132 cross linking Methods 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 9
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 3
- 230000002441 reversible effect Effects 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000002161 passivation Methods 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011949 advanced processing technology Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
-
- 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
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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 a process for reducing the specific surface area of a graphite cathode material of a lithium battery, which comprises the steps of carrying out ultrasonic crushing on asphalt powder in water by adopting an ultrasonic crushing technology, further crushing the asphalt powder into ultrafine asphalt particles with the particle size of 0.1-0.5 mu m, crushing the graphite particles into graphite powder with the particle size of 0.1-100 mu m by adopting the ultrasonic crushing technology, and then screening out spherical graphite particles with the particle size of 0.1-10 mu m, wherein the particle size of the particles processed by the ultrasonic crushing technology is generally 0.1-10 mu m compared with the prior common crushing technology, the particle size of the particles processed by adopting the traditional crushing technology is smaller, the stirring and mixing efficiency of the ultrafine asphalt particles and the spherical graphite particles is higher, the effect is better, and the specific surface area of the asphalt-based hard carbon-coated natural graphite cathode material prepared by adopting the ultrasonic crushing technology is smaller than that of the asphalt-based hard carbon-coated natural graphite cathode material prepared by adopting the traditional crushing technology, and further, the cycle performance and reversible capacity of the negative electrode material are improved more obviously, and the performance of the lithium ion battery is stronger.
Description
Technical Field
The invention relates to the field of lithium battery processing, in particular to a process for reducing the specific surface area of a graphite negative electrode material of a lithium battery.
Background
Lithium Ion Batteries (LIBs) are the best battery system in terms of comprehensive performance at present, have the characteristics of high specific energy, long cycle life, small size, light weight, no memory effect, no pollution and the like, and are rapidly developed into a new generation of energy storage power supply for power support in the fields of information technology, electric vehicles, hybrid vehicles, aerospace and the like.
The spherical graphite is modified on the surface of graphite by adopting an advanced processing technology, and produced graphite products with different fineness and similar to an ellipsoid shape belong to high-added-value deep-processed products in graphite products, have the characteristics of high conductivity, high crystallinity and low cost, high theoretical lithium intercalation capacity, low and flat charge-discharge potential, concentrated particle size distribution, large tap density, small specific surface area, stable quality and the like, are an important part currently used as a lithium ion battery cathode material, are rapidly developed in recent years for power automobiles and the like, and open up wide prospects for the application of the spherical graphite in the field of new energy.
In the first charge and discharge process of the liquid lithium ion battery, the electrode material and the electrolyte react on a solid-liquid phase interface to form a passivation layer covering the surface of the electrode material, the passivation layer is an excellent conductor of Li +, and Li + can be freely inserted and extracted through the passivation layer, so that the passivation layer is called a solid electrolyte interface film (SEI film for short), and the formation of the SEI film consumes part of lithium ions, so that the first charge and discharge irreversible capacity is increased, and the charge and discharge efficiency of the electrode material is reduced. The specific surface area of the negative electrode material can influence the generation of an SEI film, thereby influencing the performance of the lithium ion battery,
at present, some low-end negative electrode materials have large specific surface areas, and react with electrolyte to generate an SEI film in the charging and discharging processes, so that the first coulombic efficiency of the lithium ion battery is low, and in addition, the low-end negative electrode materials are easy to be co-embedded with organic solvents in the electrolyte, so that a negative electrode graphite layer is expanded and peeled off, and the electrolyte is further consumed, therefore, the invention provides a process capable of reducing the specific surface areas of the lithium battery graphite negative electrode materials to improve the working efficiency of the lithium ion battery, and is necessary.
However, the existing method for reducing the specific surface area of the graphitized material of the negative electrode of the lithium battery only crushes and mixes one of spherical graphite and asphalt particles, the crushed particle size is still large, the reduction of the specific surface area after the two are mixed is not obvious enough, and the improvement of the cycle performance and the reversible capacity of the negative electrode material is not obvious enough.
Disclosure of Invention
The invention aims to provide a process for reducing the specific surface area of a graphite negative electrode material of a lithium battery, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the process for reducing the specific surface area of the graphite negative electrode material of the lithium battery comprises the following steps of:
step 1: ultrasonic crushing of asphalt powder, ultrasonic crushing of asphalt powder in water via ultrasonic cavitation technology and further crushing of asphalt powder into superfine asphalt grains of 0.1-0.5 micron size;
step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
and step 3: processing the spherical graphite, namely pretreating a graphite raw material, crushing and spheroidizing the graphite raw material after pretreatment, classifying the crushed and spheroidized spherical graphite raw material, purifying the classified spherical graphite, and drying the purified spherical graphite;
and 4, step 4: stirring and mixing asphalt particles and spherical graphite, and mixing the crushed and dried ultrafine asphalt particles and the deeply processed spherical graphite particles according to the mass ratio of 7:100-9: 100;
and 5: heating and coating, in air atmosphere, stirring and heating the mixed material in a 300 deg.C roller furnace or horizontal kettle for 3.0 hr with air flow of 1.2m3H, completing the asphalt pairUniformly coating natural graphite and crosslinking and curing asphalt;
step 6: carbonizing, and carbonizing the heated and coated natural graphite in a pushed slab kiln or a roller kiln at 1080 ℃ to prepare the asphalt-based hard carbon coated natural graphite cathode material.
As a further scheme of the invention: the material pretreatment of the spherical graphite processing is to put the graphite raw material into a sieve for primary screening, and the screened falling graphite raw material enters a permanent magnet iron remover to remove iron and other magnetic substances in the graphite raw material.
As a still further scheme of the invention: the crushing and spheroidizing of the spherical graphite processing are implemented by pouring pretreated graphite into a crusher for crushing, then preparing the crushed graphite powder into the spherical graphite by a shaping mode, wherein the crushing period is 15 minutes/time, the crushing period is 2-4 times, sampling detection is carried out once each time the crushing period is finished, and the rotating speed of the crusher is 2000 revolutions/minute.
As a still further scheme of the invention: the classification of the processing of the spherical graphite is to pour the crushed and spheroidized graphite into a classifier to be classified and discharged, spherical graphite particles of 0.1-10um are classified, the feeding amount of the classifier is controlled at 35 kg/min, and the rotating speed of the classifier is 1200 r/min.
As a still further scheme of the invention: the purification of the processing of the spherical graphite is to repeatedly wash the initial product of the spherical graphite crystal with water to obtain a purer spherical graphite crystal.
As a still further scheme of the invention: the drying of the spherical graphite processing is to put the spherical graphite crystal into a dryer for drying, adjust the temperature inside the dryer to 80-120 ℃, and continuously heat for 3-4h to obtain the spherical graphite crystal.
As a still further scheme of the invention: the crushing comprises coarse crushing and fine crushing, wherein the pretreated graphite is poured into a coarse crusher for coarse crushing to obtain graphite particles with the particle size of 0.5-2cm, and then the graphite particles after coarse crushing are poured into a fine crusher, and the fine crusher adopts an ultrasonic crushing technology to crush the graphite particles to graphite powder with the particle size of 0.1-100 mu m.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts the ultrasonic crushing technology to carry out ultrasonic crushing on asphalt powder in water, the particle size of the asphalt powder is further crushed into ultramicro asphalt particles with the particle size of 0.1-0.5 mu m, the graphite particles are crushed into graphite powder with the particle size of 0.1-100 mu m by adopting the ultrasonic crushing technology, and then spherical graphite particles with the particle size of 0.1-10 mu m are screened out, compared with the prior common crushing technology, the particle size processed by the ultrasonic crushing technology is generally 0.1-10 mu m and is smaller than the particle size processed by the traditional crushing technology, so when the ultramicro asphalt particles and the spherical graphite particles are stirred and mixed, the mixing efficiency is higher, the mixing effect is better, compared with the asphalt-based hard carbon-coated natural graphite cathode material prepared by the traditional crushing technology, the asphalt-based hard carbon-coated natural graphite cathode material prepared by adopting the ultrasonic crushing technology has smaller specific surface area, and further, the cycle performance and reversible capacity of the negative electrode material are improved more obviously, and the performance of the lithium ion battery is stronger.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Please refer to FIG. 1
Example 1
The process for reducing the specific surface area of the graphite negative electrode material of the lithium battery comprises the following steps of:
step 1: ultrasonic crushing of asphalt powder, ultrasonic crushing of asphalt powder in water via ultrasonic cavitation technology and further crushing of asphalt powder into superfine asphalt grains of 0.1-0.5 micron size;
step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
and step 3: processing the spherical graphite, namely pretreating a graphite raw material, crushing and spheroidizing the graphite raw material after pretreatment, classifying the crushed and spheroidized spherical graphite raw material, purifying the classified spherical graphite, and drying the purified spherical graphite;
and 4, step 4: stirring and mixing asphalt particles and spherical graphite, and mixing the crushed and dried ultrafine asphalt particles and the deeply processed spherical graphite particles according to a mass ratio of 7: 100;
and 5: heating and coating, in air atmosphere, stirring and heating the mixed material in a 300 deg.C roller furnace or horizontal kettle for 3.0 hr with air flow of 1.2m3Completing uniform coating of the natural graphite by the asphalt and crosslinking and curing of the asphalt;
step 6: carbonizing, and carbonizing the heated and coated natural graphite in a pushed slab kiln or a roller kiln at 1080 ℃ to prepare the asphalt-based hard carbon coated natural graphite cathode material.
The pretreatment of the spherical graphite processing material is to put the graphite raw material into a sieve for primary screening, and the screened falling graphite raw material enters a permanent magnet iron remover to remove iron and other magnetic substances in the graphite raw material.
The crushing and spheroidizing of the spherical graphite processing is to pour the pretreated graphite into a crusher for crushing, then prepare the crushed graphite powder into the spherical graphite by a shaping mode, wherein the crushing period is 15 minutes/time, the crushing period is 2 times, sampling detection is carried out once the crushing period is finished, and the rotating speed of the crusher is 2000 revolutions per minute.
The grading of the processing of the spherical graphite is to pour the crushed and spheroidized graphite into a grader for grading and discharging, and 0.1-10um spherical graphite particles are graded, the feeding amount of the grader is controlled at 35 kg/min, and the rotating speed of the grader is 1200 r/min.
The purification of the spherical graphite processing is to repeatedly wash the initial product of the spherical graphite crystal with water to obtain a purer spherical graphite crystal.
The drying of the spherical graphite processing is to put the spherical graphite crystal into a dryer for drying, adjust the temperature inside the dryer to 80 ℃, and continuously heat for 3 hours to obtain the spherical graphite crystal.
The crushing comprises coarse crushing and fine crushing, wherein the pretreated graphite is poured into a coarse crusher for coarse crushing to obtain graphite particles with the particle size of 0.5-2cm, and then the graphite particles after coarse crushing are poured into a fine crusher which adopts an ultrasonic crushing technology to crush the graphite particles to graphite powder with the particle size of 0.1-100 mu m.
Example 2
The process for reducing the specific surface area of the graphite negative electrode material of the lithium battery comprises the following steps of:
step 1: ultrasonic crushing of asphalt powder, ultrasonic crushing of asphalt powder in water via ultrasonic cavitation technology and further crushing of asphalt powder into superfine asphalt grains of 0.1-0.5 micron size;
step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
and step 3: processing the spherical graphite, namely pretreating a graphite raw material, crushing and spheroidizing the graphite raw material after pretreatment, classifying the crushed and spheroidized spherical graphite raw material, purifying the classified spherical graphite, and drying the purified spherical graphite;
and 4, step 4: stirring and mixing asphalt particles and spherical graphite, and mixing the crushed and dried ultrafine asphalt particles and the deeply processed spherical graphite particles according to a mass ratio of 8: 100;
and 5: heating and coating, in air atmosphere, stirring and heating the mixed material in a 300 deg.C roller furnace or horizontal kettle for 3.0 hr with air flow of 1.2m3Completing uniform coating of the natural graphite by the asphalt and crosslinking and curing of the asphalt;
step 6: carbonizing, and carbonizing the heated and coated natural graphite in a pushed slab kiln or a roller kiln at 1080 ℃ to prepare the asphalt-based hard carbon coated natural graphite cathode material.
The pretreatment of the spherical graphite processing material is to put the graphite raw material into a sieve for primary screening, and the screened falling graphite raw material enters a permanent magnet iron remover to remove iron and other magnetic substances in the graphite raw material.
The crushing and spheroidizing of the spherical graphite processing is to pour the pretreated graphite into a crusher for crushing, then prepare the crushed graphite powder into the spherical graphite by a shaping mode, wherein the crushing period is 15 minutes/time, the crushing period is 3 times, sampling detection is carried out once the crushing period is finished, and the rotating speed of the crusher is 2000 revolutions per minute.
The grading of the processing of the spherical graphite is to pour the crushed and spheroidized graphite into a grader for grading and discharging, and 0.1-10um spherical graphite particles are graded, the feeding amount of the grader is controlled at 35 kg/min, and the rotating speed of the grader is 1200 r/min.
The purification of the spherical graphite processing is to repeatedly wash the initial product of the spherical graphite crystal with water to obtain a purer spherical graphite crystal.
The drying of the spherical graphite processing is to put the spherical graphite crystal into a dryer for drying, adjust the temperature inside the dryer to 100 ℃, and continuously heat for 3.5 hours to obtain the spherical graphite crystal.
The crushing comprises coarse crushing and fine crushing, wherein the pretreated graphite is poured into a coarse crusher for coarse crushing to obtain graphite particles with the particle size of 0.5-2cm, and then the graphite particles after coarse crushing are poured into a fine crusher which adopts an ultrasonic crushing technology to crush the graphite particles to graphite powder with the particle size of 0.1-100 mu m.
Example 3
The process for reducing the specific surface area of the graphite negative electrode material of the lithium battery comprises the following steps of:
step 1: ultrasonic crushing of asphalt powder, ultrasonic crushing of asphalt powder in water via ultrasonic cavitation technology and further crushing of asphalt powder into superfine asphalt grains of 0.1-0.5 micron size;
step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
and step 3: processing the spherical graphite, namely pretreating a graphite raw material, crushing and spheroidizing the graphite raw material after pretreatment, classifying the crushed and spheroidized spherical graphite raw material, purifying the classified spherical graphite, and drying the purified spherical graphite;
and 4, step 4: stirring and mixing asphalt particles and spherical graphite, and mixing the crushed and dried ultrafine asphalt particles and the deeply processed spherical graphite particles according to a mass ratio of 9: 100;
and 5: heating and coating, in air atmosphere, stirring and heating the mixed material in a 300 deg.C roller furnace or horizontal kettle for 3.0 hr with air flow of 1.2m3Completing uniform coating of the natural graphite by the asphalt and crosslinking and curing of the asphalt;
step 6: carbonizing, and carbonizing the heated and coated natural graphite in a pushed slab kiln or a roller kiln at 1080 ℃ to prepare the asphalt-based hard carbon coated natural graphite cathode material.
The pretreatment of the spherical graphite processing material is to put the graphite raw material into a sieve for primary screening, and the screened falling graphite raw material enters a permanent magnet iron remover to remove iron and other magnetic substances in the graphite raw material.
The crushing and spheroidizing of the spherical graphite processing is to pour the pretreated graphite into a crusher for crushing, then prepare the crushed graphite powder into the spherical graphite by a shaping mode, wherein the crushing period is 15 minutes/time, the crushing period is 4 times, sampling detection is carried out once the crushing period is finished, and the rotating speed of the crusher is 2000 revolutions per minute.
The grading of the processing of the spherical graphite is to pour the crushed and spheroidized graphite into a grader for grading and discharging, and 0.1-10um spherical graphite particles are graded, the feeding amount of the grader is controlled at 35 kg/min, and the rotating speed of the grader is 1200 r/min.
The purification of the spherical graphite processing is to repeatedly wash the initial product of the spherical graphite crystal with water to obtain a purer spherical graphite crystal.
The spherical graphite is dried by putting the spherical graphite crystal into a dryer, adjusting the temperature inside the dryer to 120 ℃, and continuously heating for 4 hours to obtain the spherical graphite crystal.
The crushing comprises coarse crushing and fine crushing, wherein the pretreated graphite is poured into a coarse crusher for coarse crushing to obtain graphite particles with the particle size of 0.5-2cm, and then the graphite particles after coarse crushing are poured into a fine crusher which adopts an ultrasonic crushing technology to crush the graphite particles to graphite powder with the particle size of 0.1-100 mu m.
By testing the specific surface area of the products obtained in the three examples, the specific surface area of the product obtained in the third example is the smallest, so the process effect is the best by adopting the process in the example 3.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (7)
1. The process for reducing the specific surface area of the graphite cathode material of the lithium battery is characterized by comprising the following steps of: the method comprises the following steps:
step 1: ultrasonic crushing of asphalt powder, ultrasonic crushing of asphalt powder in water via ultrasonic cavitation technology and further crushing of asphalt powder into superfine asphalt grains of 0.1-0.5 micron size;
step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
and step 3: processing the spherical graphite, namely pretreating a graphite raw material, crushing and spheroidizing the graphite raw material after pretreatment, classifying the crushed and spheroidized spherical graphite raw material, purifying the classified spherical graphite, and drying the purified spherical graphite;
and 4, step 4: stirring and mixing asphalt particles and spherical graphite, and mixing the crushed and dried ultrafine asphalt particles and the deeply processed spherical graphite particles according to the mass ratio of 7:100-9: 100;
and 5: heating and coating, in air atmosphere, stirring and heating the mixed material in a 300 deg.C roller furnace or horizontal kettle for 3.0 hr with air flow of 1.2m3H, completing asphalt paradiseThen uniformly coating graphite and crosslinking and curing asphalt;
step 6: carbonizing, and carbonizing the heated and coated natural graphite in a pushed slab kiln or a roller kiln at 1080 ℃ to prepare the asphalt-based hard carbon coated natural graphite cathode material.
2. The process for reducing the specific surface area of the graphite negative electrode material of the lithium battery as claimed in claim 1, wherein: the material pretreatment of the spherical graphite processing is to put the graphite raw material into a sieve for primary screening, and the screened falling graphite raw material enters a permanent magnet iron remover to remove iron and other magnetic substances in the graphite raw material.
3. The process for reducing the specific surface area of the graphite negative electrode material of the lithium battery as claimed in claim 1, wherein: the crushing and spheroidizing of the spherical graphite processing are implemented by pouring pretreated graphite into a crusher for crushing, then preparing the crushed graphite powder into the spherical graphite by a shaping mode, wherein the crushing period is 15 minutes/time, the crushing period is 2-4 times, sampling detection is carried out once each time the crushing period is finished, and the rotating speed of the crusher is 2000 revolutions/minute.
4. The process for reducing the specific surface area of the graphite negative electrode material of the lithium battery as claimed in claim 1, wherein: the classification of the processing of the spherical graphite is to pour the crushed and spheroidized graphite into a classifier to be classified and discharged, spherical graphite particles of 0.1-10um are classified, the feeding amount of the classifier is controlled at 35 kg/min, and the rotating speed of the classifier is 1200 r/min.
5. The process for reducing the specific surface area of the graphite negative electrode material of the lithium battery as claimed in claim 1, wherein: the purification of the processing of the spherical graphite is to repeatedly wash the initial product of the spherical graphite crystal with water to obtain a purer spherical graphite crystal.
6. The process for reducing the specific surface area of the graphite negative electrode material of the lithium battery as claimed in claim 1, wherein: the drying of the spherical graphite processing is to put the spherical graphite crystal into a dryer for drying, adjust the temperature inside the dryer to 80-120 ℃, and continuously heat for 3-4h to obtain the spherical graphite crystal.
7. The process for reducing the specific surface area of the graphite negative electrode material of the lithium battery as claimed in claim 3, wherein: the crushing comprises coarse crushing and fine crushing, wherein the pretreated graphite is poured into a coarse crusher for coarse crushing to obtain graphite particles with the particle size of 0.5-2cm, and then the graphite particles after coarse crushing are poured into a fine crusher, and the fine crusher adopts an ultrasonic crushing technology to crush the graphite particles to graphite powder with the particle size of 0.1-100 mu m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210159883.5A CN114512652B (en) | 2022-02-22 | 2022-02-22 | Process for reducing specific surface area of graphite cathode material of lithium battery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210159883.5A CN114512652B (en) | 2022-02-22 | 2022-02-22 | Process for reducing specific surface area of graphite cathode material of lithium battery |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114512652A true CN114512652A (en) | 2022-05-17 |
| CN114512652B CN114512652B (en) | 2024-04-26 |
Family
ID=81553661
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210159883.5A Active CN114512652B (en) | 2022-02-22 | 2022-02-22 | Process for reducing specific surface area of graphite cathode material of lithium battery |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114512652B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4361097A1 (en) * | 2022-09-29 | 2024-05-01 | Ningde Amperex Technology Ltd. | Composite material and preparation method thereof, electrochemical device, and electronic device |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008025188A1 (en) * | 2006-08-22 | 2008-03-06 | Btr Energy Materials Co., Ltd. | A silicon-carbon composite negative material for lithium ion battery and the preparation method of the same |
| CN104201343A (en) * | 2014-08-27 | 2014-12-10 | 宁夏共享新能源材料有限公司 | Method for reducing specific surface area of spherical graphite |
| CN105810921A (en) * | 2016-06-06 | 2016-07-27 | 田东 | Preparation method of tin-based cathode material of high-capacity lithium-ion battery |
| CN106299373A (en) * | 2016-09-20 | 2017-01-04 | 新乡市华鑫电源材料有限公司 | A kind of lithium ion battery high magnification negative material and preparation method thereof |
| CN109205611A (en) * | 2018-08-21 | 2019-01-15 | 大同新成新材料股份有限公司 | A kind of preparation process of graphite cathode material |
| CN110137449A (en) * | 2019-04-24 | 2019-08-16 | 漳州巨铭石墨材料有限公司 | A kind of modified negative electrode material of lithium ion battery and its method of modifying |
| CN110289417A (en) * | 2019-06-26 | 2019-09-27 | 鞍山赛欧新材料科技有限公司 | A kind of artificial graphite cathode material for lithium ion batteries preparation method |
| CN112573517A (en) * | 2020-12-03 | 2021-03-30 | 铜仁学院 | Preparation method of asphalt-based hard carbon-coated natural graphite negative electrode material |
-
2022
- 2022-02-22 CN CN202210159883.5A patent/CN114512652B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008025188A1 (en) * | 2006-08-22 | 2008-03-06 | Btr Energy Materials Co., Ltd. | A silicon-carbon composite negative material for lithium ion battery and the preparation method of the same |
| CN104201343A (en) * | 2014-08-27 | 2014-12-10 | 宁夏共享新能源材料有限公司 | Method for reducing specific surface area of spherical graphite |
| CN105810921A (en) * | 2016-06-06 | 2016-07-27 | 田东 | Preparation method of tin-based cathode material of high-capacity lithium-ion battery |
| CN106299373A (en) * | 2016-09-20 | 2017-01-04 | 新乡市华鑫电源材料有限公司 | A kind of lithium ion battery high magnification negative material and preparation method thereof |
| CN109205611A (en) * | 2018-08-21 | 2019-01-15 | 大同新成新材料股份有限公司 | A kind of preparation process of graphite cathode material |
| CN110137449A (en) * | 2019-04-24 | 2019-08-16 | 漳州巨铭石墨材料有限公司 | A kind of modified negative electrode material of lithium ion battery and its method of modifying |
| CN110289417A (en) * | 2019-06-26 | 2019-09-27 | 鞍山赛欧新材料科技有限公司 | A kind of artificial graphite cathode material for lithium ion batteries preparation method |
| CN112573517A (en) * | 2020-12-03 | 2021-03-30 | 铜仁学院 | Preparation method of asphalt-based hard carbon-coated natural graphite negative electrode material |
Non-Patent Citations (1)
| Title |
|---|
| 肖海河等: "沥青炭包覆微晶石墨用作锂离子电池负极材料的研究", 《功能材料》, vol. 44, no. 19, 22 September 2013 (2013-09-22), pages 2759 - 2763 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4361097A1 (en) * | 2022-09-29 | 2024-05-01 | Ningde Amperex Technology Ltd. | Composite material and preparation method thereof, electrochemical device, and electronic device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114512652B (en) | 2024-04-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106169582B (en) | A kind of natural needle coke composite graphite negative electrode material production method | |
| CN109970052B (en) | Method for granulating and secondary coating modification of natural graphite | |
| CN110474032A (en) | It is a kind of to be given up the silicon-carbon cathode material and preparation method thereof of silicon based on photovoltaic | |
| CN103811758B (en) | A kind of preparation method of synthetic graphite particle negative material | |
| CN110137449A (en) | A kind of modified negative electrode material of lithium ion battery and its method of modifying | |
| CN102800852A (en) | Preparation method of negative electrode material of power lithium-ion battery | |
| CN105731427A (en) | Lithium ion battery graphite anode material and preparation method thereof | |
| CN111509192B (en) | Method for recycling positive electrode material from waste lithium battery, obtained product and application | |
| CN110203923A (en) | A kind of lithium ion battery negative material and preparation method thereof | |
| CN109390579B (en) | Preparation method of dry-method and wet-method carbon-coated high-nickel ternary cathode material | |
| CN114620707A (en) | Preparation method of long-cycle lithium ion battery cathode material | |
| CN114512652B (en) | Process for reducing specific surface area of graphite cathode material of lithium battery | |
| CN110550635B (en) | Preparation method of novel carbon-coated silica negative electrode material | |
| CN110518203A (en) | Compound soft carbon negative electrode material and preparation method thereof, lithium ion battery | |
| CN113023724A (en) | Preparation method of high-rate graphite negative electrode material for lithium ion power battery | |
| CN103311521A (en) | Surface-modified graphite negative electrode material, and preparation method and application thereof | |
| CN102214821B (en) | Surface-modified graphitized intermediate-phase carbon micropowder and preparation method thereof | |
| CN115911633A (en) | Regeneration method of lithium ion battery graphite cathode and regenerated graphite | |
| CN219156517U (en) | Device for preparing artificial graphite negative electrode material for lithium ion battery | |
| CN110649345A (en) | Method for recycling waste lead paste in production process of lead-acid storage battery and application of recycled materials | |
| CN113526956B (en) | Low-cost long-circulation graphite negative electrode material and preparation method and application thereof | |
| CN112390252B (en) | Carbon impurity-based negative electrode material, preparation method thereof and lithium ion battery | |
| CN113363466A (en) | Low-cost graphite negative electrode material based on crucible crushed aggregates and preparation method thereof | |
| CN109524627B (en) | SiOx negative electrode material with controllable oxygen content, preparation method and lithium ion battery | |
| CN112652767A (en) | Preparation method of soft carbon negative electrode material of lithium ion battery |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |