CN106477569A - A kind of preprocess method of artificial graphite material and products obtained therefrom and application - Google Patents
A kind of preprocess method of artificial graphite material and products obtained therefrom and application Download PDFInfo
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- CN106477569A CN106477569A CN201510896782.6A CN201510896782A CN106477569A CN 106477569 A CN106477569 A CN 106477569A CN 201510896782 A CN201510896782 A CN 201510896782A CN 106477569 A CN106477569 A CN 106477569A
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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
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
This discloses a kind of preprocess method of artificial graphite material and products obtained therefrom and application, the preprocess method of described artificial graphite material, comprises the steps：1. the artificial graphite material that D50 is 10 24 μm is dried to moisture therein percentage ratio≤1% accounting for material gross mass, obtains dry artificial graphite material；2. by the artificial graphite material of the drying of step 1 gained at a high speed modified fusion machine with rotating speed batch mixing 5 30min of 1300 1700r/min, sieve afterwards and obtain product；The present invention also provides the artificial graphite material being prepared by the preprocess method of described artificial graphite material and its is preparing the application in cell negative electrode material, this preprocess method can improve the isotropic degree of Delanium, the quick charge characteristic of lifting Delanium, improve the regular appearance degree of material, and do not affect the trend of the original particle size distribution of material, do not affect the performance of capacity and efficiency, artificial graphite material safety after process is good, stable in properties, does not almost have difference between batch.
Description
Technical field
The present invention relates to graphite manufactures field, specifically a kind of preprocess method of artificial graphite material and products obtained therefrom and application.
Background technology
Universalness with lithium ion battery applications, mobile phone, panel computer, electric automobile, electric tool etc. are stepping up to the demand of lithium ion battery, the world in this networking, electronization, the usage degree more and more higher to electronic products such as mobile phones for the people, almost arrive mobile phone not from the degree of handss, and in the so fast world of rhythm, a lithium ion battery being capable of quick charge will become a new focus；Currently available technology have been directed towards improve battery performance carried out widely studied, however as the raising further that battery rapid charging performance is required, need to improve the isotropic degree of Delanium, reduce the OI value of material, the quick charge characteristic of lifting Delanium, thus improve the overall material property of Delanium；Although artificial graphite material has higher first charge-discharge efficiency, excellent cycle performance, but the charge/discharge capacity of general Delanium is all relatively low, for improving the capacity of Delanium, need to make Delanium have higher degree of graphitization, but also therefore make Delanium anisotropic degree improve a lot, so that the rapid charge characteristic of Delanium is deteriorated, lead to it to use and be restricted；Delanium, in process of manufacture, typically has the operation of crushing and classification simultaneously, and the production process of crushing and classification influences whether the particle size distribution of material, and the processing abrasion of machine influences whether synthetic graphite particles' pattern, so that drawing abillity is deteriorated；The numerous studies surface of lithium ion battery negative material, the isotropic degree of material and rapid charge characteristic have certain relation, and that is, the isotropic degree of material is higher, rapid charge characteristic is better, conversely, the isotropic degree of material is lower, rapid charge characteristic is poorer；The isotropic degree of material is represented with OI value, OI value=004 peak area/110 peak area, and wherein 004 peak area and 110 peak areas are to be obtained with XRD test；For improving the isotropic degree of Delanium, prior art or the degree of graphitization by reducing Delanium, or the OI value reducing material is processed by pelletize, although these technology can reduce the OI value of material, but therefore or reduce the capacity of Delanium, or make the poor processability of Delanium, therefore need a kind of processing method, the method can improve the isotropic degree of Delanium while keeping the high graphitization degree of Delanium.
Content of the invention
It is an object of the invention to provide a kind of preprocess method of artificial graphite material and products obtained therefrom and application are to overcome the defect that in prior art, high power capacity artificial graphite material isotropic degree is low, rapid charge characteristic is poor, to solve the problems, such as to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme：
A kind of preprocess method of artificial graphite material, comprises the steps：
1) by D50, the artificial graphite material for 10-24 μm is dried to moisture therein percentage ratio≤1% accounting for material gross mass, obtains dry artificial graphite material；
2) by the artificial graphite material of the drying of step 1 gained at a high speed modified fusion machine with the rotating speed batch mixing 5-30min of 1300-1700r/min, sieve afterwards and obtain product.
As the further scheme of the present invention：Described artificial graphite material is the conventional various commonly artificial graphite raw material in this area；It is preferred that the D50 value of described artificial graphite material is 14-22 μm；Described D50 is volume average particle size, and the cumulative particle sizes percentile referring to a sample reaches corresponding particle diameter when 50%, and its physical significance is that particle diameter is more than its granule and accounts for 50%, also accounts for 50% less than its granule.
As the present invention further scheme：The single treatment amount of the artificial graphite material described in step 1 is 5-20kg, more preferably for 10-15kg.
As the present invention further scheme：The drying of the artificial graphite material described in step 1 is the conventional drying process in this area, carries out typically in drying baker；The time of described drying is preferably 1-4 hour, more preferably for 2-3 hour；Preferably 100-500 DEG C of the temperature of described drying, more preferably for 200-300 DEG C.
As the present invention further scheme：Batch mixing described in step 2 is preferably with the rotating speed batch mixing 5-25min of 1300-1600r/min, before batch mixing, preferably also includes the machine to batch mixing and carries out clearing up, detects, not have other impurities to be preferred.
As the present invention further scheme：Artificial graphite material described in step 2 obtains finished product after sieving, and the mesh number sieved is 200-250 mesh, more preferably for 250 mesh, to remove impurity and bulky grain.
As the present invention further scheme：Artificial graphite material described in step 2 obtains finished product after sieving, and the artificial graphite material of gained before actual use, preferably also can routinely be processed in step censorship.
As the present invention further scheme：The artificial graphite material that the preprocess method of foregoing artificial graphite material is obtained.
As the present invention further scheme：Application in preparing cell negative electrode material for the artificial graphite material product that the preprocess method of foregoing artificial graphite material is obtained, described cell negative electrode material is preferably lithium ion battery negative material.
On the basis of meeting common sense in the field, above-mentioned each optimum condition, can combination in any, obtain final product the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material are all commercially available.
Compared with prior art, the invention has the beneficial effects as follows：The artificial graphite material preprocess method simple possible of the present invention is it is adaptable to industrialized production；The artificial graphite material of the preparation of the present invention has advantages below：OI value substantially reduces；Overall particle size distribution will not be impacted；Regular appearance degree increases, modification more uniform, do not affect the performance of capacity and efficiency；Stable in properties, does not almost have difference between batch；The artificial graphite material preprocess method of the present invention both can improve the isotropic degree of Delanium, and the rapid charge characteristic of lifting Delanium is moreover it is possible to improve the processing characteristics of Delanium；And do not affect the trend of the original particle size distribution of material, do not affect the performance of capacity and efficiency.
Brief description
Fig. 1 is the raw meal particle size scattergram of embodiment 2 before processing in the present invention.
Fig. 2 is the material electron microscope of embodiment 2 before processing in the present invention.
Fig. 3 is the material electron microscope after embodiment 2 process in the present invention.
Specific embodiment
Further illustrate the present invention below by the mode of embodiment, but therefore do not limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or selects according to catalogue.
The Delanium class product that used in following embodiments, artificial graphite material produces for Shanghai Shanshan Science and Technology Co., Ltd.
Embodiment 1
Artificial graphite material (is designated as raw material A), and the particle diameter D50 of commodity mark is 20 μm about, the common 12Kg of raw material, detection sample before pretreatment, and its D50 particle diameter is 20.3 μm, and OI value is 3.6, and tap density is 0.82g/cm3.
The preprocess method of artificial graphite material, comprises the steps：
(1) artificial graphite material is put in drying baker, through 300 DEG C of dried 2 hours, account for percentage ratio≤1% of material gross mass to moisture；
(2) check that whether normal the equipment of fusion machine run, cleaning fusion machine is it is ensured that free from admixture；The particle diameter D50 of 12Kg drying is that 20.3 μm of artificial graphite material put into batch mixing in the modified fusion machine of high speed, the time is 10 minutes, rotating speed 1300r/m；Material sieves process afterwards, crosses grit number 250 mesh, obtains finished product.
After testing, material particle diameter after treatment is 20.3 μm, and OI value is 3.2, and tap density is 0.85g/cm3.
Embodiment 2
Artificial graphite material (is designated as raw material B), and the particle diameter D50 of commodity mark is 16 μm about, the common 12Kg of raw material, detection sample before pretreatment, and its D50 particle diameter is 16.0 μm, and OI value is 3.5, and tap density is 0.90g/cm3.
The preprocess method of artificial graphite material, comprises the steps：
(1) artificial graphite material is put in drying baker, through 300 DEG C of dried 2 hours, account for percentage ratio≤1% of material gross mass to moisture；
(2) check that whether normal the equipment of fusion machine run, cleaning fusion machine is it is ensured that free from admixture；The particle diameter D50 of 12Kg drying is that 16.0 μm of artificial graphite material put into batch mixing in the modified fusion machine of high speed, the time is 10 minutes, rotating speed 1300r/m；Material sieves process afterwards, crosses grit number 250 mesh, obtains finished product.
After testing, material particle diameter after treatment is 16.0 μm, and OI value is 3.1, and tap density is 0.94g/cm3.
Embodiment 3
Artificial graphite material (is designated as raw material A), and the particle diameter D50 of commodity mark is 20 μm about, the common 12Kg of raw material, detection sample before pretreatment, and its D50 particle diameter is 20.3 μm, and OI value is 3.6, and tap density is 0.82g/cm3.
The preprocess method of artificial graphite material, comprises the steps：
(1) artificial graphite material is put in drying baker, through 300 DEG C of dried 2 hours, account for percentage ratio≤1% of material gross mass to moisture；
(2) check that whether normal the equipment of fusion machine run, cleaning fusion machine is it is ensured that free from admixture；The particle diameter D50 of 12Kg drying is that 20.3 μm of artificial graphite material put into batch mixing in the modified fusion machine of high speed, the time is 20 minutes, rotating speed 1300r/m；Material sieves process afterwards, crosses grit number 250 mesh, obtains finished product.
After testing, material particle diameter after treatment is 20.3 μm, and OI value is 2.5, and tap density is 0.88g/cm3.
Embodiment 4
Artificial graphite material (is designated as raw material B), and the particle diameter D50 of commodity mark is 16 μm about, the common 12Kg of raw material, detection sample before pretreatment, and its D50 particle diameter is 16.0 μm, and OI value is 3.5, and tap density is 0.90g/cm3.
The preprocess method of artificial graphite material its comprise the steps：
(1) artificial graphite material is put in drying baker, through 300 DEG C of dried 2 hours, account for percentage ratio≤1% of material gross mass to moisture；
(2) check that whether normal the equipment of fusion machine run, cleaning fusion machine is it is ensured that free from admixture；The particle diameter D50 of 12Kg drying is that 16.0 μm of artificial graphite material put into batch mixing in the modified fusion machine of high speed, the time is 20 minutes, rotating speed 1300r/m；Material sieves process afterwards, crosses grit number 250 mesh, obtains finished product.
After testing, material particle diameter after treatment is 16.0 μm, and OI value is 2.4, and tap density is 0.97g/cm3.
Embodiment 5
Artificial graphite material (is designated as raw material B), and the particle diameter D50 of commodity mark is 16 μm about, the common 12Kg of raw material, detection sample before pretreatment, and its D50 particle diameter is 16.0 μm, and OI value is 3.5, and tap density is 0.90g/cm3.
The preprocess method of artificial graphite material, comprises the steps：
(1) artificial graphite material is put in drying baker, through 300 DEG C of dried 2 hours, account for percentage ratio≤1% of material gross mass to moisture；
(2) check that whether normal the equipment of fusion machine run, cleaning fusion machine is it is ensured that free from admixture；The particle diameter D50 of 12Kg drying is that 16.0 μm of artificial graphite material put into batch mixing in the modified fusion machine of high speed, the time is 20 minutes, rotating speed 1500r/m；Material sieves process afterwards, crosses grit number 250 mesh, obtains finished product.
After testing, material particle diameter after treatment is 16.0 μm, and OI value is 1.8, and tap density is 1.02g/cm3.
Comparative example 1
Artificial graphite material (is designated as raw material A), and the particle diameter D50 of commodity mark is 20 μm about, the common 12Kg of raw material, detection sample before pretreatment, and its D50 particle diameter is 20.3 μm, and OI value is 3.6, and tap density is 0.82g/cm3.
The preprocess method of artificial graphite material, comprises the steps：
(1) artificial graphite material is put in drying baker, through 300 DEG C of dried 2 hours, account for percentage ratio≤1% of material gross mass to moisture；
(2) check that whether normal the equipment of fusion machine run, cleaning fusion machine is it is ensured that free from admixture；The particle diameter D50 of 12Kg drying is that 20.3 μm of artificial graphite material put into batch mixing in the modified fusion machine of high speed, the time is 5 minutes, rotating speed 1300r/m；Material sieves process afterwards, crosses grit number 250 mesh, obtains finished product.
After testing, material particle diameter after treatment is 20.3 μm, and OI value is 3.6, and tap density is 0.82g/cm3.
Comparative example 2
Artificial graphite material (is designated as raw material B), and the particle diameter D50 of commodity mark is 16 μm about, the common 12Kg of raw material, detection sample before pretreatment, and its D50 particle diameter is 16.0 μm, and OI value is 3.5, and tap density is 0.90g/cm3.
The preprocess method of artificial graphite material, comprises the steps：
(1) artificial graphite material is put in drying baker, through 300 DEG C of dried 2 hours, account for percentage ratio≤1% of material gross mass to moisture；
(2) check that whether normal the equipment of fusion machine run, cleaning fusion machine is it is ensured that free from admixture；The particle diameter D50 of 12Kg drying is that 16.0 μm of artificial graphite material put into batch mixing in the modified fusion machine of high speed, the time is 5 minutes, rotating speed 1300r/m；Material sieves process afterwards, crosses grit number 250 mesh, obtains finished product.
After testing, material particle diameter after treatment is 16.0 μm, and OI value is 3.5, and tap density is 0.90g/cm3.
Comparative example 3
Artificial graphite material (is designated as raw material B), and the particle diameter D50 of commodity mark is 16 μm about, the common 12Kg of raw material, detection sample before pretreatment, and its D50 particle diameter is 16.0 μm, and OI value is 3.5, and tap density is 0.90g/cm3.
The preprocess method of artificial graphite material, comprises the steps：
(1) artificial graphite material is put in drying baker, through 300 DEG C of dried 2 hours, account for percentage ratio≤1% of material gross mass to moisture；
(2) check that whether normal the equipment of fusion machine run, cleaning fusion machine is it is ensured that free from admixture；The particle diameter D50 of 12Kg drying is that 16.0 μm of artificial graphite material put into batch mixing in the modified fusion machine of high speed, the time is 8 minutes, rotating speed 1300r/m；Material sieves process afterwards, crosses grit number 250 mesh, obtains finished product.
After testing, material particle diameter after treatment is 16.0 μm, and OI value is 3.5, and tap density is 0.90g/cm3.
Effect example
Artificial graphite material in embodiment 1-5 and comparative example 1-3 is carried out respectively with particle diameter, OI value, tap density and ash grade an index test；Discharge capacity and the test of first charge-discharge efficiency are carried out using half-cell method of testing to the artificial graphite material in embodiment 1-5 and comparative example 1-3；Also carry out sieving performance detection simultaneously, and result is all listed in table 1.
The used instrument title of present invention test and model：
Particle diameter D50：Laser fineness gage MS2000；
OI value：XRD D8ADVANCE；
Ash：High-temperature electric resistance furnace SX2-2.5-12；
Tap density, FZS4-4B tap density analyzer；
Assay method national standard：Tap density GB/T5162-2006/ISO3953:1993；
Used by present invention test, half-cell test instrunment and method are：Make 2430 type batteries, graphite sample, the N-Methyl pyrrolidone containing 6～7% Kynoar and conductive black mix in proportion, and are applied on Copper Foil, the pole piece coating is put into temperature standby for being vacuum dried 4 hours in 110 DEG C of vacuum drying ovens；Simulated battery is assemblied in the German Braun glove box of applying argon gas and carries out, electrolyte is 1M LiPF6+EC: EMC: DMC=1: 1: 1 (volume ratio), metal lithium sheet is to electrode, and electrochemical property test is carried out on U.S. ArbinBT2000 type cell tester.
Discharge and recharge system：
1) constant-current discharge (0.6mA, 0.005V)；
2) stand (10min)；
3) constant-current charge (0.05mA, 0.005V)；
4) stand (10min)；
5) constant-current discharge (0.6mA, 2.000V).
Sieve method for testing performance：Screen cloth being converted into funnel-form so as to encase beaker mouth, and be enclosed within beaker mouth with rubber band makes it fix, and the slurry mixing is poured on a little screen cloth (200 mesh), is gently extruded with spoon, observes slurry and sieves what state；If cannot sieve, then change the less screen cloth of mesh number, if 100 mesh still cannot sieve, no longer sieve, then see the need of coating depending on concrete condition, after choosing suitable screen cloth, slurry is poured on screen cloth, is gently extruded with spoon, slowly make slurry flow into following beaker, screen cloth can be rinsed with water when should be noted oversize, then observe whether oversize has the phenomenons such as bulky grain.
The performance parameter of the artificial graphite material of each embodiment such as table 1.
The performance parameter of the artificial graphite material of each embodiment of table 1
As can be seen from Table 1：Embodiment 1 and embodiment 2, the artificial graphite material after this method is processed, OI value is reduced to 3.2 and 3.1 by original 3.6 and 3.5, and tap density is also by 0.82g/cm simultaneously3And 0.90g/cm3It is respectively increased 0.85g/cm3And 0.94g/cm3, discharge capacity and first efficiency are not affected, and performance of sieving also makes moderate progress；Embodiment 3 and enforcement 4, artificial graphite material after this method is processed, it is more that prolongation process time can make the OI value of material reduce, and tap density improves more, OI value is reduced to 2.5 and 2.4 by original 3.6 and 3.5, and tap density is also by 0.82g/cm simultaneously3And 0.90g/cm3It is respectively increased 0.88g/cm3And 0.97g/cm3, discharge capacity and first efficiency are not affected, and performance of sieving also makes moderate progress；Embodiment 5 increase fusion treatment rotating speed it is also possible to make material OI value reduce more, tap density raising more, OI value is reduced to 1.8 by original 3.5, and tap density is also by 0.90g/cm simultaneously3Bring up to 1.02g/cm3, discharge capacity and first efficiency are not affected, and performance of sieving also makes moderate progress；Comparative example 1-3 reduces fusion machine rotating speed, reduces process time and the OI value of artificial graphite material is not improved.
Refer to Fig. 1-3, specifically, from the Delanium raw material of embodiment 2 and the particle size distribution figure of the artificial graphite material being obtained and its Electronic Speculum shape appearance figure, after before processing, the particle size distribution of material does not change significantly, and the artificial graphite material pattern after process is more regular.
Above the better embodiment of this patent is explained in detail, but this patent is not limited to above-mentioned embodiment, in the ken that one skilled in the relevant art possesses, can also make a variety of changes on the premise of without departing from this patent objective.
Claims (10)
1. a kind of preprocess method of artificial graphite material is it is characterised in that comprise the steps：
1) by D50, the artificial graphite material for 10-24 μm is dried and accounts for the hundred of material gross mass to moisture therein
Divide ratio≤1%, obtain dry artificial graphite material；
2) by the artificial graphite material of the drying of step 1 gained at a high speed modified fusion machine with 1300-1700
The rotating speed batch mixing 5-30min of r/min, sieves afterwards and obtains product.
2. the preprocess method of artificial graphite material according to claim 1 is it is characterised in that step
The D50 value of the artificial graphite material described in 1 is 14-22 μm.
3. the preprocess method of artificial graphite material according to claim 1 is it is characterised in that step 1
The single treatment amount of described artificial graphite material is 5-20kg.
4. the preprocess method of artificial graphite material according to claim 1 is it is characterised in that step 1
The single treatment amount of described artificial graphite material is 10-15kg.
5. the preprocess method of artificial graphite material according to claim 1 is it is characterised in that step 1
Described artificial graphite material drying time is 1-4 hour；Described artificial graphite material baking temperature is
100-500℃.
6. the preprocess method of artificial graphite material according to claim 1 is it is characterised in that step 1
Described artificial graphite material drying time is 2-3 hour；Described artificial graphite material baking temperature is
200-300℃.
7. the preprocess method of artificial graphite material according to claim 1 is it is characterised in that step 2
Described batch mixing is the rotating speed batch mixing 5-25min with 1300-1600r/min.
8. the preprocess method of artificial graphite material according to claim 1 is it is characterised in that step 2
Described artificial graphite material obtains finished product after sieving, and the mesh number sieved is 200-250 mesh.
9. the artificial stone that the preprocess method of the artificial graphite material as described in any one of claim 1～8 is obtained
Ink material product.
10. application in preparing cell negative electrode material for the artificial graphite material product as claimed in claim 9.
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| CN110492066A (en) * | 2019-08-01 | 2019-11-22 | 深圳市比克动力电池有限公司 | A kind of anode plate for lithium ionic cell of quick charge and preparation method thereof |
| CN111916670A (en) * | 2020-09-23 | 2020-11-10 | 珠海冠宇电池股份有限公司 | Negative plate and application thereof |
| WO2021109133A1 (en) * | 2019-12-06 | 2021-06-10 | 宁德时代新能源科技股份有限公司 | Secondary battery and device containing same |
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