CN114512652B - Process for reducing specific surface area of graphite cathode material of lithium battery - Google Patents
Process for reducing specific surface area of graphite cathode material of lithium battery Download PDFInfo
- Publication number
- CN114512652B CN114512652B CN202210159883.5A CN202210159883A CN114512652B CN 114512652 B CN114512652 B CN 114512652B CN 202210159883 A CN202210159883 A CN 202210159883A CN 114512652 B CN114512652 B CN 114512652B
- Authority
- CN
- China
- Prior art keywords
- graphite
- asphalt
- grinding
- 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.)
- Active
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 172
- 239000010439 graphite Substances 0.000 title claims abstract description 172
- 238000000034 method Methods 0.000 title claims abstract description 38
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 19
- 239000010406 cathode material Substances 0.000 title claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 85
- 239000002245 particle Substances 0.000 claims abstract description 83
- 239000010426 asphalt Substances 0.000 claims abstract description 69
- 238000005516 engineering process Methods 0.000 claims abstract description 24
- 229910021382 natural graphite Inorganic materials 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 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
- 239000002994 raw material Substances 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 25
- 238000012545 processing Methods 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 239000013078 crystal Substances 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 15
- 238000000576 coating method Methods 0.000 claims description 15
- 239000007773 negative electrode material Substances 0.000 claims description 12
- 238000010000 carbonizing Methods 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 239000010405 anode material Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000004132 cross linking Methods 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 239000000203 mixture Substances 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
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 3
- 230000002441 reversible effect Effects 0.000 abstract description 3
- 239000003792 electrolyte Substances 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 3
- 238000002161 passivation Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 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
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram 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
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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
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 grinding on asphalt powder in water by adopting an ultrasonic grinding technology, further grinding the asphalt powder into ultra-micro asphalt particles with the particle size of 0.1-0.5 mu m, grinding the graphite particles into graphite powder with the particle size of 0.1-100 mu m by adopting the ultrasonic grinding technology, then screening out spherical graphite particles with the particle size of 0.1-10 mu m, wherein the particle size processed by the ultrasonic grinding technology is generally 0.1-10 mu m, compared with the particle size processed by the traditional grinding technology, the particle size of the particles processed by the ultrasonic grinding technology is smaller, the stirring and mixing efficiency of the ultra-micro asphalt particles and the spherical graphite particles is higher, the effect is better, and compared with the asphalt-based hard carbon coated natural graphite cathode material prepared by adopting the ultrasonic grinding technology, the specific surface area of the asphalt-based hard carbon coated natural graphite cathode material is smaller, so that the cycle performance and reversible capacity of the cathode material are more obviously improved, 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
Along with the progress of economic globalization and the continuous rise of energy demands, the search of new energy storage devices has become a focus of attention in the related fields of new energy, lithium Ion Batteries (LIB) are battery systems with the best comprehensive performance at present, have the characteristics of high specific energy, long cycle life, small volume, light weight, no memory effect, no pollution and the like, and rapidly develop into new generation energy storage power supplies for power support in the fields of information technology, electric vehicles, hybrid vehicles, aerospace and the like.
The spherical graphite adopts advanced processing technology to modify the graphite surface, and the produced graphite has different fineness and is similar to the shape
The elliptic graphite product belongs to a deep-processing product with high added value in the graphite product, has the characteristics of high conductivity, high crystallinity, low cost, high theoretical lithium intercalation capacity, low charge and discharge potential, flatness, concentrated particle size distribution, large tap density, small specific surface area, stable quality and the like, is an important part of the lithium ion battery cathode material at present, and opens up a wide prospect for the application of the elliptic graphite product in the field of new energy due to the rapid development of power automobiles and the like in recent years.
In the first charge and discharge process of the liquid lithium ion battery, the electrode material reacts with the electrolyte on the solid-liquid phase interface to form a passivation layer covering the surface of the electrode material, and the passivation layer is an excellent conductor of Li+ which can be freely inserted and extracted through the passivation layer, so that the solid electrolyte interface film is called SEI film for short, part of lithium ions are consumed by the formation of the SEI film, the irreversible capacity of the first charge and discharge is increased, and the charge and discharge efficiency of the electrode material is reduced. The specific surface area of the cathode material can influence the generation of SEI film, thereby influencing the performance of the lithium ion battery,
At present, a few low-end negative electrode materials have large specific surface area, and react with electrolyte to generate an SEI film in the charge and discharge process, so that the lithium ion battery has low coulomb efficiency for the first time, and in addition, the lithium ion battery is easy to have co-intercalation with an organic solvent in the electrolyte, which can cause expansion and peeling of a negative electrode graphite layer and further consume the electrolyte, so that the process capable of reducing the specific surface area of the graphite negative electrode material of the lithium ion battery is invented to improve the working efficiency of the lithium ion battery, and is very necessary.
However, the existing method for reducing the specific surface area of the lithium battery cathode graphitized material only comprises the steps of crushing and mixing one of spherical graphite and asphalt particles, and the crushed particle size is still larger, so that the reduction of the specific surface area is not obvious enough after the spherical graphite and the asphalt particles are mixed, and the cycle performance and the reversible capacity of the cathode material are not obviously improved.
Disclosure of Invention
The invention aims to provide a process for reducing the specific surface area of a graphite anode material of a lithium battery, so as to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the process for reducing the specific surface area of the graphite cathode material of the lithium battery comprises the following steps:
step 1: ultrasonic grinding of asphalt powder, ultrasonic grinding of asphalt powder in water by ultrasonic cavitation technology, and further crushing the particle size of the asphalt powder into ultrafine asphalt particles of 0.1-0.5 mu m;
Step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
Step 3: the method comprises the steps of (1) processing spherical graphite, pre-treating a graphite raw material, crushing and spheroidizing the graphite raw material after pre-treating, grading the crushed and spheroidized spherical graphite raw material, purifying the graded spherical graphite, and drying the purified spherical graphite;
Step 4: mixing asphalt particles and spherical graphite by stirring, and mixing crushed and dried ultrafine asphalt particles and deep-processed spherical graphite particles according to the mass ratio of 7:100-9:100;
Step 5: heating and coating, namely heating the mixture in a roller furnace or a horizontal kettle at 300 ℃ under the air atmosphere while stirring, wherein the heating time is 3.0h, and the air flow is 1.2m 3/h, so as to finish uniform coating of asphalt on natural graphite and crosslinking and curing of asphalt;
step 6: carbonizing, namely carbonizing the natural graphite subjected to heating coating in a push plate kiln or a roller kiln at 1080 ℃ to obtain the asphalt-based hard carbon coated natural graphite anode material.
As a further scheme of the invention: the pretreatment of the material for processing the spherical graphite is to put the graphite raw material into a sieve for preliminary screening, and the screened graphite raw material falls into a permanent magnet iron remover to remove iron and other magnetic substances in the graphite raw material.
As still further aspects of the invention: the grinding and spheroidizing process of the spherical graphite comprises the steps of pouring pretreated graphite into a grinder for grinding, then preparing the ground graphite powder into spherical graphite in a shaping mode, wherein the grinding period is 15 minutes/time, the grinding period is 2-4 times, sampling detection is carried out every time the grinding period is finished, and the rotating speed of the grinder is 2000 revolutions/minute.
As still further aspects of the invention: the classification of the spherical graphite processing is to pour the crushed and spheroidized graphite into a classifier for classification and discharge, and the spherical graphite particles with the granularity of 0.1-10 mu m are classified, wherein the feeding amount of the classifier is controlled at 35 kg/min, and the rotating speed of the classifier is 1200 r/min.
As still further aspects of the invention: the purification of the spherical graphite processing is to repeatedly wash an initial product of the spherical graphite crystal with water to obtain purer spherical graphite crystal.
As still further aspects of the invention: and the spherical graphite is dried by putting the spherical graphite crystal into a dryer, adjusting the temperature in the dryer to 80-120 ℃, and continuously heating for 3-4 hours to obtain the spherical graphite crystal.
As still further aspects of the invention: the grinding comprises coarse grinding and fine grinding, wherein the pretreated graphite is poured into a coarse grinding machine to be subjected to coarse grinding, the coarse grinding is carried out to obtain graphite particles with the granularity of 0.5-2cm, then the graphite particles after the coarse grinding are poured into a fine grinding machine, and the fine grinding machine adopts an ultrasonic grinding technology to grind the graphite particles into graphite powder with the granularity of 0.1-100 mu m.
Compared with the prior art, the invention has the beneficial effects that:
According to the invention, the asphalt powder is subjected to ultrasonic crushing in water by adopting an ultrasonic crushing technology, the particle size of the asphalt powder is further crushed into ultrafine 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 conventional common crushing technology, the particle size of the particles processed by adopting the ultrasonic crushing technology is generally 0.1-10 mu m, and is smaller than the particle size processed by adopting the conventional crushing technology, so that when the ultrafine asphalt particles and the spherical graphite particles are stirred and mixed, the mixing efficiency is higher, the mixing effect is better, and compared with the asphalt-based hard carbon coated natural graphite negative electrode material prepared by adopting the ultrasonic crushing technology, the specific surface area of the asphalt-based hard carbon coated natural graphite negative electrode material is smaller, so that the cycle performance and reversible capacity of the negative electrode material are improved more obviously, and the performance of a lithium ion battery is stronger.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Please refer to fig. 1
Examples
The process for reducing the specific surface area of the graphite cathode material of the lithium battery comprises the following steps:
step 1: ultrasonic grinding of asphalt powder, ultrasonic grinding of asphalt powder in water by ultrasonic cavitation technology, and further crushing the particle size of the asphalt powder into ultrafine asphalt particles of 0.1-0.5 mu m;
Step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
Step 3: the method comprises the steps of (1) processing spherical graphite, pre-treating a graphite raw material, crushing and spheroidizing the graphite raw material after pre-treating, grading the crushed and spheroidized spherical graphite raw material, purifying the graded spherical graphite, and drying the purified spherical graphite;
Step 4: mixing asphalt particles and spherical graphite by stirring, and mixing crushed and dried ultrafine asphalt particles and deep-processed spherical graphite particles according to a mass ratio of 7:100;
Step 5: heating and coating, namely heating the mixture in a roller furnace or a horizontal kettle at 300 ℃ under the air atmosphere while stirring, wherein the heating time is 3.0h, and the air flow is 1.2m 3/h, so as to finish uniform coating of asphalt on natural graphite and crosslinking and curing of asphalt;
step 6: carbonizing, namely carbonizing the natural graphite subjected to heating coating in a push plate kiln or a roller kiln at 1080 ℃ to obtain the asphalt-based hard carbon coated natural graphite anode material.
The pretreatment of the material for processing the spherical graphite is to put the graphite raw material into a sieve for preliminary screening, and the screened graphite raw material falls into a permanent magnet iron remover to remove iron and other magnetic substances in the graphite raw material.
The grinding and spheroidizing process of the spherical graphite comprises the steps of pouring pretreated graphite into a grinder for grinding, then preparing the ground graphite powder into spherical graphite in a shaping mode, wherein the grinding period is 15 minutes/time, the grinding period is 2 times, sampling detection is carried out every time the grinding period is finished, and the rotating speed of the grinder is 2000 revolutions/minute.
The classification of the spherical graphite processing is to pour the crushed and spheroidized graphite into a classifier for classification and discharge, and the spherical graphite particles with the granularity of 0.1-10 mu m are classified, wherein the feeding amount of the classifier is controlled at 35 kg/min, and the rotating speed of the classifier is 1200 r/min.
The purification of the spherical graphite processing is to repeatedly wash an initial product of the spherical graphite crystal with water to obtain purer spherical graphite crystal.
And the drying of the spherical graphite processing is to put the spherical graphite crystal into a dryer for drying, the temperature in the dryer is adjusted to 80 ℃, and the spherical graphite crystal is obtained after continuous heating for 3 hours.
The grinding comprises coarse grinding and fine grinding, wherein the pretreated graphite is poured into a coarse grinder to carry out coarse grinding, the coarse grinding is carried out to obtain graphite particles with the granularity of 0.5-2cm, then the graphite particles after the coarse grinding are poured into a fine grinder, and the fine grinder adopts an ultrasonic grinding technology to grind the graphite particles into graphite powder with the granularity of 0.1-100 mu m.
Examples
The process for reducing the specific surface area of the graphite cathode material of the lithium battery comprises the following steps:
step 1: ultrasonic grinding of asphalt powder, ultrasonic grinding of asphalt powder in water by ultrasonic cavitation technology, and further crushing the particle size of the asphalt powder into ultrafine asphalt particles of 0.1-0.5 mu m;
Step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
Step 3: the method comprises the steps of (1) processing spherical graphite, pre-treating a graphite raw material, crushing and spheroidizing the graphite raw material after pre-treating, grading the crushed and spheroidized spherical graphite raw material, purifying the graded spherical graphite, and drying the purified spherical graphite;
Step 4: mixing asphalt particles and spherical graphite by stirring, and mixing crushed and dried ultrafine asphalt particles and deep-processed spherical graphite particles according to a mass ratio of 8:100;
Step 5: heating and coating, namely heating the mixture in a roller furnace or a horizontal kettle at 300 ℃ under the air atmosphere while stirring, wherein the heating time is 3.0h, and the air flow is 1.2m 3/h, so as to finish uniform coating of asphalt on natural graphite and crosslinking and curing of asphalt;
step 6: carbonizing, namely carbonizing the natural graphite subjected to heating coating in a push plate kiln or a roller kiln at 1080 ℃ to obtain the asphalt-based hard carbon coated natural graphite anode material.
The pretreatment of the material for processing the spherical graphite is to put the graphite raw material into a sieve for preliminary screening, and the screened graphite raw material falls into a permanent magnet iron remover to remove iron and other magnetic substances in the graphite raw material.
The grinding and spheroidizing process of the spherical graphite comprises the steps of pouring pretreated graphite into a grinder for grinding, then preparing the ground graphite powder into spherical graphite in a shaping mode, wherein the grinding period is 15 minutes/time, the grinding period is 3 times, sampling detection is carried out every time the grinding period is finished, and the rotating speed of the grinder is 2000 revolutions/minute.
The classification of the spherical graphite processing is to pour the crushed and spheroidized graphite into a classifier for classification and discharge, and the spherical graphite particles with the granularity of 0.1-10 mu m are classified, wherein the feeding amount of the classifier is controlled at 35 kg/min, and the rotating speed of the classifier is 1200 r/min.
The purification of the spherical graphite processing is to repeatedly wash an initial product of the spherical graphite crystal with water to obtain purer spherical graphite crystal.
And the drying of the spherical graphite processing is to put the spherical graphite crystal into a dryer for drying, the temperature in the dryer is adjusted to 100 ℃, and the spherical graphite crystal is obtained after continuous heating for 3.5 hours.
The grinding comprises coarse grinding and fine grinding, wherein the pretreated graphite is poured into a coarse grinder to carry out coarse grinding, the coarse grinding is carried out to obtain graphite particles with the granularity of 0.5-2cm, then the graphite particles after the coarse grinding are poured into a fine grinder, and the fine grinder adopts an ultrasonic grinding technology to grind the graphite particles into graphite powder with the granularity of 0.1-100 mu m.
Examples
The process for reducing the specific surface area of the graphite cathode material of the lithium battery comprises the following steps:
step 1: ultrasonic grinding of asphalt powder, ultrasonic grinding of asphalt powder in water by ultrasonic cavitation technology, and further crushing the particle size of the asphalt powder into ultrafine asphalt particles of 0.1-0.5 mu m;
Step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
Step 3: the method comprises the steps of (1) processing spherical graphite, pre-treating a graphite raw material, crushing and spheroidizing the graphite raw material after pre-treating, grading the crushed and spheroidized spherical graphite raw material, purifying the graded spherical graphite, and drying the purified spherical graphite;
Step 4: mixing asphalt particles and spherical graphite by stirring, and mixing crushed and dried ultrafine asphalt particles and deep-processed spherical graphite particles according to a mass ratio of 9:100;
Step 5: heating and coating, namely heating the mixture in a roller furnace or a horizontal kettle at 300 ℃ under the air atmosphere while stirring, wherein the heating time is 3.0h, and the air flow is 1.2m 3/h, so as to finish uniform coating of asphalt on natural graphite and crosslinking and curing of asphalt;
step 6: carbonizing, namely carbonizing the natural graphite subjected to heating coating in a push plate kiln or a roller kiln at 1080 ℃ to obtain the asphalt-based hard carbon coated natural graphite anode material.
The pretreatment of the material for processing the spherical graphite is to put the graphite raw material into a sieve for preliminary screening, and the screened graphite raw material falls into a permanent magnet iron remover to remove iron and other magnetic substances in the graphite raw material.
The grinding and spheroidizing process of the spherical graphite comprises the steps of pouring pretreated graphite into a grinder for grinding, then preparing the ground graphite powder into spherical graphite in a shaping mode, wherein the grinding period is 15 minutes/time, the grinding period is 4 times, sampling detection is carried out every time the grinding period is finished, and the rotating speed of the grinder is 2000 revolutions/minute.
The classification of the spherical graphite processing is to pour the crushed and spheroidized graphite into a classifier for classification and discharge, and the spherical graphite particles with the granularity of 0.1-10 mu m are classified, wherein the feeding amount of the classifier is controlled at 35 kg/min, and the rotating speed of the classifier is 1200 r/min.
The purification of the spherical graphite processing is to repeatedly wash an initial product of the spherical graphite crystal with water to obtain purer spherical graphite crystal.
And the drying of the spherical graphite processing is to put the spherical graphite crystal into a dryer for drying, the temperature in the dryer is adjusted to 120 ℃, and the spherical graphite crystal is obtained after continuous heating for 4 hours.
The grinding comprises coarse grinding and fine grinding, wherein the pretreated graphite is poured into a coarse grinder to carry out coarse grinding, the coarse grinding is carried out to obtain graphite particles with the granularity of 0.5-2cm, then the graphite particles after the coarse grinding are poured into a fine grinder, and the fine grinder adopts an ultrasonic grinding technology to grind the graphite particles into graphite powder with the granularity of 0.1-100 mu m.
By testing the specific surface areas of the products obtained in the three examples, the specific surface area of the product obtained in the third example is the smallest, so that the process effect of the example 3 is the best.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present 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 grinding of asphalt powder, ultrasonic grinding of asphalt powder in water by ultrasonic cavitation technology, and further crushing the particle size of the asphalt powder into ultrafine asphalt particles of 0.1-0.5 mu m;
Step 2: drying the ultrafine asphalt particles, and then putting the crushed ultrafine asphalt particles into a dryer for drying;
Step 3: the method comprises the steps of (1) processing spherical graphite, pre-treating a graphite raw material, crushing and spheroidizing the graphite raw material after pre-treating, grading the crushed and spheroidized spherical graphite raw material, purifying the graded spherical graphite, and drying the purified spherical graphite;
Step 4: mixing asphalt particles and spherical graphite by stirring, and mixing crushed and dried ultrafine asphalt particles and deep-processed spherical graphite particles according to the mass ratio of 7:100-9:100;
Step 5: heating and coating, namely heating the mixture in a roller furnace or a horizontal kettle at 300 ℃ under the air atmosphere while stirring, wherein the heating time is 3.0h, and the air flow is 1.2m 3/h, so as to finish uniform coating of asphalt on natural graphite and crosslinking and curing of asphalt;
step 6: carbonizing, namely carbonizing the natural graphite subjected to heating coating in a push plate kiln or a roller kiln at 1080 ℃ to obtain the asphalt-based hard carbon coated natural graphite anode material.
2. The process for reducing the specific surface area of a graphite negative electrode material of a lithium battery according to claim 1, wherein the process comprises the following steps: the pretreatment of the material for processing the spherical graphite is to put the graphite raw material into a sieve for preliminary screening, and the screened graphite raw material falls into 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 a graphite negative electrode material of a lithium battery according to claim 1, wherein the process comprises the following steps: the grinding and spheroidizing process of the spherical graphite comprises the steps of pouring pretreated graphite into a grinder for grinding, then preparing the ground graphite powder into spherical graphite in a shaping mode, wherein the grinding period is 15 minutes/time, the grinding period is 2-4 times, sampling detection is carried out every time the grinding period is finished, and the rotating speed of the grinder is 2000 revolutions/minute.
4. The process for reducing the specific surface area of a graphite negative electrode material of a lithium battery according to claim 1, wherein the process comprises the following steps: the classification of the spherical graphite processing is to pour the crushed and spheroidized graphite into a classifier for classification and discharge, and the spherical graphite particles with the granularity of 0.1-10 mu m are classified, wherein 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 a graphite negative electrode material of a lithium battery according to claim 1, wherein the process comprises the following steps: the purification of the spherical graphite processing is to repeatedly wash an initial product of the spherical graphite crystal with water to obtain purer spherical graphite crystal.
6. The process for reducing the specific surface area of a graphite negative electrode material of a lithium battery according to claim 1, wherein the process comprises the following steps: and the spherical graphite is dried by putting the spherical graphite crystal into a dryer, adjusting the temperature in the dryer to 80-120 ℃, and continuously heating for 3-4 hours to obtain the spherical graphite crystal.
7. The process for reducing the specific surface area of a graphite negative electrode material of a lithium battery according to claim 3, wherein: the grinding comprises coarse grinding and fine grinding, wherein the pretreated graphite is poured into a coarse grinding machine to be subjected to coarse grinding, the coarse grinding is carried out to obtain graphite particles with the granularity of 0.5-2cm, then the graphite particles after the coarse grinding are poured into a fine grinding machine, and the fine grinding machine adopts an ultrasonic grinding technology to grind the graphite particles into graphite powder with the granularity 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 CN114512652A (en) | 2022-05-17 |
| CN114512652B true 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) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115425215A (en) * | 2022-09-29 | 2022-12-02 | 宁德新能源科技有限公司 | Composite material, method for producing same, 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 |
|---|
| 沥青炭包覆微晶石墨用作锂离子电池负极材料的研究;肖海河等;《功能材料》;20130922;第44卷(第19期);第2759-2763页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114512652A (en) | 2022-05-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106169582B (en) | A kind of natural needle coke composite graphite negative electrode material production method | |
| 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 | |
| CN102195036B (en) | Surface modified graphitized interphase carbon micro-powder and preparation method thereof | |
| CN103811758B (en) | A kind of preparation method of synthetic graphite particle negative material | |
| CN109970052B (en) | Method for granulating and secondary coating modification of natural graphite | |
| CN106784741B (en) | Carbon-silicon composite material, preparation method thereof and lithium ion battery containing composite material | |
| CN109860548B (en) | Preparation method and application of nano silicon material | |
| CN111509192B (en) | Method for recycling positive electrode material from waste lithium battery, obtained product and application | |
| CN104733705A (en) | Negative pole material for lithium ion power cell and preparation method thereof | |
| CN110203923A (en) | A kind of lithium ion battery negative material and preparation method thereof | |
| CN112652770A (en) | Silicon-carbon negative electrode material with low specific surface area and preparation method thereof | |
| CN105789627A (en) | Preparation method of high-performance graphite negative electrode material for lithium ion battery | |
| CN114512652B (en) | Process for reducing specific surface area of graphite cathode material of lithium battery | |
| CN109390579B (en) | Preparation method of dry-method and wet-method carbon-coated high-nickel ternary cathode material | |
| CN111342015B (en) | High-compaction low-resistance lithium iron phosphate and preparation method thereof | |
| CN110212184A (en) | A kind of prelithiation method of carbon negative electrode material of lithium ion cell | |
| CN102214821B (en) | Surface-modified graphitized intermediate-phase carbon micropowder and preparation method thereof | |
| 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 | |
| CN114551799A (en) | Negative electrode slurry and preparation method thereof, negative electrode plate and lithium ion battery | |
| CN109879286B (en) | Preparation method of lithium battery silicon-carbon negative electrode composite material | |
| CN112652767A (en) | Preparation method of soft carbon negative electrode material of lithium ion battery | |
| CN109524627B (en) | SiOx negative electrode material with controllable oxygen content, preparation method and lithium ion battery | |
| CN111755681A (en) | Silicon-carbon negative electrode material for lithium ion battery and preparation method thereof | |
| CN117727915B (en) | Silicon-carbon composite material with micro silicon crystal size and preparation method and application thereof |
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 |