CN103879997B - The preprocess method and products obtained therefrom of a kind of artificial graphite material and application - Google Patents
The preprocess method and products obtained therefrom of a kind of artificial graphite material and application Download PDFInfo
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- CN103879997B CN103879997B CN201210563268.7A CN201210563268A CN103879997B CN 103879997 B CN103879997 B CN 103879997B CN 201210563268 A CN201210563268 A CN 201210563268A CN 103879997 B CN103879997 B CN 103879997B
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Abstract
The invention discloses a kind of preprocess methods of artificial graphite material, which is characterized in that it includes the following steps：（1）The D50 artificial graphite materials for being 16 22 μm are dried to moisture therein to percentage≤2% for accounting for material gross mass, obtain dry artificial graphite material；（2）By step（1）The artificial graphite material of the drying of gained, with 3 30min of rotating speed batch mixing of 1700 2200r/min, is sieved later in the modified fusion machine of high speed.The artificial graphite material being prepared the present invention also provides the preprocess method by the artificial graphite material and its application in preparing cell negative electrode material.The tap density of the artificial graphite material of the present invention significantly improves；Overall particle size distribution will not be impacted, and size particles distribution ground is evenly；Regular appearance degree increases, and modification ground is more complete uniform, does not influence the performance of capacity and efficiency；Property is stablized, almost without difference between batch.
Description
Technical field
The present invention relates to a kind of preprocess method of artificial graphite material and products obtained therefrom and applications.
Background technology
In recent years, more stringent requirements are proposed for performance of the universalness of electronic device to secondary cell.Especially lithium ion
The sudden emergence of battery, compared with ni-Cd or Ni-MH battery, using lithium ion battery with higher energy density and preferably
Performance.Have at present very much, however as to the further of battery performance requirements for the research for improving battery performance
It improves, it is also necessary to the compacted density of battery is improved, to more greatly improve the material property of artificial graphite entirety.
Artificial graphite material has processing performance well, but there are the lower defects of compacted density.Artificial stone
Ink material generally has the program of subsequent processing classification during production and processing, and the production routine for processing classification is logical
Often influence whether the size distribution of material, simultaneously because in process machine abrasion, also affect of artificial graphite
Particle shape looks, and then the compacted density of material entirety can be made to reduce.
In lithium ion battery design process, compacted density=surface density/(pole piece roll after thickness-afflux body thickness),
Unit：g/cm3；In the production process, compacted density has large effect to lithium-ion-power cell to battery performance.It is general next
Say, compacted density is bigger, the capacity of battery can do it is higher, so compacted density is the important ginseng of battery material energy density
Examine one of index.Compacted density not only has relationship with the size of particle, density, and also and the pattern of particle has relationship, compacted density
Big generally has good particle normal distribution.It is believed that under conditions of process conditions are certain, compacted density is bigger, electricity
The capacity in pond is higher.
The method for improving artificial graphite compacted density at present is mainly to improve the degree of graphitization of material, the raising of degree of graphitization
Material can be made softer, it is more preferable to press, to improve the compacted density of artificial graphite.But the degree of graphitization of material is improved merely
Material can only be made softer, the pattern of particle can't be changed, the overall particle size distribution of particle does not have big change, therefore is compacted
Than relatively limited, which solves the raising degree of density.
Invention content
The technical problem to be solved by the present invention is to the particle surface amendments in order to overcome existing artificial graphite material not
It improves and without the subsequent processings such as sieving defect that causes compacted density not high, and a kind of powder of raising artificial graphite material is provided
Last compacted density, but the performance of the original size distribution of material and capacity and efficiency is not influenced, while the pattern of material being made to advise
Whole degree increases, and safety is good, and property is stablized, the preprocess method almost without the artificial graphite material of difference and institute between batch
Obtain product and application.
One of technical solution provided by the invention is：A kind of preprocess method of artificial graphite material comprising Xia Shubu
Suddenly：
（1）By D50 be 16-22 μm of artificial graphite material dry to moisture therein account for the percentage of material gross mass≤
2%, obtain dry artificial graphite material；
（2）By step（1）The artificial graphite material of the drying of gained is in the modified fusion machine of high speed with 1700-2200r/
The rotating speed batch mixing 3-30min of min is sieved later.
In the present invention, step（1）The artificial graphite material is the various common artificial graphite former materials of this field routine
Material；Preferably, the D50 values of the artificial graphite material are 18-21 μm.The D50 is volume average particle size, refers to a sample
The cumulative particle sizes percentile of product reaches grain size corresponding when 50%, and physical significance is that grain size is accounted for more than its particle
50%, the particle less than it also accounts for 50%.
In the present invention, step（1）The single treatment amount of the artificial graphite material is preferably 1.5-3kg, more preferably
It is most preferably 2kg for 2-2.5kg.
In the present invention, step（1）The drying is the drying process of this field routine, is carried out generally in drying box；
The time of the drying is preferably 1-3 hours, is more preferably 1.5-3 hours；The temperature of the drying is preferably
100-150 DEG C, be more preferably 120-150 DEG C, is most preferably 150 DEG C.
In the present invention, step（2）The batch mixing is preferably with the rotating speed batch mixing 10-20min of 1800-2000r/min.
Before the batch mixing, further includes preferably being cleared up the machine of batch mixing, being detected, be preferred with no other impurities.
In the present invention, step（2）The mesh number of the sieving is preferably 200-250 mesh, is more preferably 250 mesh, to remove
Impurity and bulky grain.
In the present invention, in step（2）After the sieving, the artificial graphite material of gained before actual use, compared with
It can also routinely step inspection handle goodly.
Technical solution provided by the invention second is that：People made from the preprocess method of foregoing artificial graphite material
Make graphite material.
The three of technical solution provided by the invention are：People made from the preprocess method of foregoing artificial graphite material
Make application of the graphite material in preparing cell negative electrode material.
In the present invention, the cell negative electrode material is preferably lithium ion battery negative material.
On the basis of common knowledge of the art, above-mentioned each optimum condition can be combined arbitrarily to get each preferable reality of the present invention
Example.
The reagents and materials used in the present invention are commercially available.
The positive effect of the present invention is that：The compacted density of the artificial graphite material of the present invention significantly improves；Material
Granule-morphology it is more regular, overall particle size distribution trend will not be more they tended to normal distribution by large effect, size distribution；
The no big change of the physical and chemical index of material, does not influence the performance of capacity and efficiency；Material properties is stablized, between batch almost
There is no difference；Simple production process is feasible, easy to operate, is suitable for industrialized production.
Description of the drawings
Fig. 1 is the particle size distribution figure before 2 sample treatment of embodiment.
Fig. 2 is the particle size distribution figure after 2 sample treatment of embodiment.
Fig. 3 is the electron microscope before and after 2 sample treatment of embodiment, wherein（a）For the Electronic Speculum before 2 sample treatment of embodiment point
Butut,（b）For Electronic Speculum distribution map after 2 sample treatment of embodiment.
Specific implementation mode
It is further illustrated the present invention below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions, or according to quotient
Product specification selects.
Embodiment 1
Artificial graphite material（It is denoted as raw material A）, the D50 of commodity mark is 16 μm or so, and the total 2kg of raw material, sample is being handled
The volume average particle size D50 of preceding detection is 16.4 μm, real density 2.24g/cm3, compacted density 1.49g/cm3。
（1）Artificial graphite material is put into drying box and is dried 1.5 hours through 150 DEG C, until moisture therein accounts for object
Expect percentage≤2% of gross mass；
（2）Check whether the equipment operation of fusion machine is normal, clears up fusion machine, it is ensured that free from admixture；It is 16.4 by 2kg D50
μm artificial graphite material be put into batch mixing in the modified fusion machine of high speed, the time is 3 minutes, rotating speed 1700r/m；Later by material
Sieving is handled, and it is 250 mesh to cross grit number.
After testing, the grain size for artificial graphite material that treated is 16.0 μm, real density 2.24g/cm3, compacted density
1.56g/cm3。
Embodiment 2
Artificial graphite material（It is denoted as raw material B）, the D50 of commodity mark is 18 μm or so, and the total 2kg of raw material, sample is being handled
The volume average particle size D50 of preceding detection is 18.2 μm, real density 2.25g/cm3, compacted density 1.47g/cm3。
（1）Artificial graphite material is put into drying box and is dried 1.5 hours through 150 DEG C, until moisture therein accounts for object
Expect percentage≤2% of gross mass；
（2）Check whether the equipment operation of fusion machine is normal, clears up fusion machine, it is ensured that free from admixture；It is by 2.5kg D50
18.2 μm of artificial graphite material is put into batch mixing in the modified fusion machine of high speed, and the time is 5 minutes, rotating speed 1700r/m；Later by object
Material carries out sieving processing, crosses 250 mesh of grit number.
After testing, 17.5 μm of the grain size for artificial graphite material that treated, real density 2.25g/cm3, compacted density
1.61g/cm3。
Embodiment 3
Artificial graphite material（It is denoted as raw material A）, the D50 of commodity mark is 16 μm or so, and the total 2.5kg of raw material, sample is being located
The volume average particle size D50 detected before reason is 16.4 μm, real density 2.24g/cm3, compacted density 1.49g/cm3。
（1）Artificial graphite material is put into drying box and is dried 2.0 hours through 150 DEG C, until moisture therein accounts for object
Expect percentage≤2% of gross mass；
（2）Check whether the equipment operation of fusion machine is normal, clears up fusion machine, it is ensured that free from admixture；It is 16.4 by 2kg D50
μm artificial graphite material be put into batch mixing in the modified fusion machine of high speed, the time is 10 minutes, rotating speed 1800r/m；Later by object
Expect sieving processing, crosses 250 mesh of grit number.
After testing, 15.4 μm of the grain size for artificial graphite material that treated, real density 2.24g/cm3, compacted density
1.68g/cm3。
Embodiment 4
Artificial graphite material（It is denoted as raw material B）, the D50 of commodity mark is 18 μm or so, and the total 2kg of raw material, sample is being handled
The volume average particle size D50 of preceding detection is 18.2 μm, real density 2.25g/cm3, compacted density 1.47g/cm3。
（1）Artificial graphite material is put into drying box and is dried 1.5 hours through 120 DEG C, until moisture therein accounts for object
Percentage≤2% for expecting gross mass, it is in dry fine-powdered to make material integrally；
（2）Check whether the equipment operation of batch mixer is normal, clears up batch mixer, it is ensured that free from admixture；It is 18.2 by 2kg D50
μm artificial graphite material be put into batch mixing in the modified fusion machine of high speed, the time is 10 minutes, rotating speed 1900r/m；Later by material
Sieving is handled, and crosses 250 mesh of grit number.
After testing, 16.6 μm of the grain size for artificial graphite material that treated, real density 2.25g/cm3, compacted density
1.74g/cm3。
Embodiment 5
Artificial graphite material（It is denoted as raw material B）, the D50 of commodity mark is 18 μm or so, and the total 3kg of raw material, sample is being handled
The volume average particle size D50 of preceding detection is 18.2 μm, real density 2.25g/cm3, compacted density 1.47g/cm3。
（1）Artificial graphite material is put into drying box and is dried 1.5 hours through 150 DEG C, until moisture therein accounts for object
Percentage≤2% for expecting gross mass, it is in dry fine-powdered to make material integrally；
（2）Check whether the equipment operation of fusion machine is normal, clears up fusion machine, it is ensured that free from admixture；It is 18.2 by 2kg D50
μm artificial graphite material be put into batch mixing in the modified fusion machine of high speed, the time is 20 minutes, rotating speed 2000r/m；Later by material
Sieving is handled, and crosses 200 mesh of grit number.
After testing, the grain size for artificial graphite material that treated is 15.2 μm, real density 2.25g/cm3, compacted density
1.80g/cm3。
Embodiment 6
Artificial graphite material（It is denoted as raw material A）, the D50 of commodity mark is 16 μm or so, and the total 1.5kg of raw material, sample is being located
The volume average particle size D50 detected before reason is 16.0 μm, real density 2.24g/cm3, compacted density 1.47g/cm3。
（1）Artificial graphite material is put into drying box and is dried 3 hours through 100 DEG C, until moisture therein accounts for material
Percentage≤2% of gross mass；
（2）Check whether the equipment operation of fusion machine is normal, clears up fusion machine, it is ensured that free from admixture；It is 16.0 by 2kg D50
μm artificial graphite material be put into batch mixing in the modified fusion machine of high speed, the time is 15 minutes, rotating speed 1900r/m；Later by object
Expect sieving processing, it is 250 mesh to cross grit number.
After testing, the grain size for artificial graphite material that treated is 16.0 μm, real density 2.24g/cm3, compacted density
1.67g/cm3。
Embodiment 7
Artificial graphite material（It is denoted as raw material B）, the D50 of commodity mark is 21 μm or so, and the total 2kg of raw material, sample is being handled
The volume average particle size D50 of preceding detection is 22.0 μm, real density 2.25g/cm3, compacted density 1.45g/cm3。
（1）Artificial graphite material is put into drying box and is dried 1.0 hours through 150 DEG C, until moisture therein accounts for object
Percentage≤2% for expecting gross mass, it is in dry fine-powdered to make material integrally；
（2）Check whether the equipment operation of fusion machine is normal, clears up fusion machine, it is ensured that free from admixture；It is 22.0 by 2kg D50
μm artificial graphite material be put into batch mixing in the modified fusion machine of high speed, the time is 30 minutes, rotating speed 2200r/m；Later by material
Sieving is handled, and crosses 250 mesh of grit number.
After testing, the grain size for artificial graphite material that treated is 21.8 μm, real density 2.25g/cm3, compacted density
1.81g/cm3。
Comparative example 1
Artificial graphite material（It is denoted as raw material A）, the D50 of commodity mark is 16 μm or so, and the total 2kg of raw material, sample is being handled
The volume average particle size D50 of preceding detection is 16.4 μm, real density 2.24g/cm3, compacted density 1.49g/cm3。
（1）Artificial graphite material is put into drying box and is dried 1.5 hours through 150 DEG C；
（2）Check whether the equipment operation of fusion machine is normal, clears up fusion machine, it is ensured that free from admixture；It is 16.4 by 2kg D50
μm artificial graphite material is put into batch mixing in the modified fusion machine of high speed, and the time is 3 minutes, rotating speed 1500r/m；Material is sieved later
250 mesh of grit number is crossed in processing.
After testing, the grain size for artificial graphite material that treated is 16.3 μm, real density 2.24g/cm3, compacted density
1.49g/cm3。
Comparative example 2
Artificial graphite material（It is denoted as raw material B）, the D50 of commodity mark is 18 μm or so, and the total 2kg of raw material, sample is being handled
The volume average particle size D50 of preceding detection is 18.2 μm, real density 2.25g/cm3, compacted density 1.47g/cm3。
（1）Artificial graphite material is put into drying box and is dried 1.5 hours through 150 DEG C；
（2）Check whether the equipment operation of fusion machine is normal, clears up batch mixer, it is ensured that free from admixture；It is by 2.5kg D50
18.2 μm of artificial graphite materials are put into batch mixing in the modified fusion machine of high speed, and the time is 1 minute, rotating speed 1700r/m；Later by material
Sieving is handled, and crosses 250 mesh of grit number.
After testing, 18.1 μm of the grain size for artificial graphite material that treated, real density 2.25g/cm3, compacted density
1.47g/cm3。
Comparative example 3
Artificial graphite material（It is denoted as raw material A）, the D50 of commodity mark is 16 μm or so, and the total 2kg of raw material, sample is being handled
The volume average particle size D50 of preceding detection is 16.4 μm, real density 2.24g/cm3, compacted density 1.49g/cm3。
（1）Artificial graphite material is put into drying box and is dried 2.0 hours through 150 DEG C；
（2）Check whether the equipment operation of fusion machine is normal, clears up fusion machine, it is ensured that free from admixture；It is 16.4 by 2kg D50
μm artificial graphite material is put into batch mixing in the modified fusion machine of high speed, and the time is 1 minute, rotating speed 1500r/m；Material is sieved later
250 mesh of grit number is crossed in processing.
After testing, 16.2 μm of the grain size for artificial graphite material that treated, real density 2.24g/cm3, compacted density
1.49g/cm3。
Effect example
Artificial plumbago negative pole material in embodiment 1 ~ 5 and comparative example 1 ~ 3 is carried out respectively grain size, real density, compacting it is close
Degree and ash grade an index test；Electric discharge appearance is carried out to the artificial graphite material in embodiment 1 ~ 5 using half-cell test method
The test of amount and first charge-discharge efficiency, is as a result listed in table 1.Sieving performance detection is also carried out simultaneously, is as a result listed in table
2。
Instrument title and model used in test are as follows：
Laser fineness gage：MS2000, Dandong Bai Te Instrument Ltd. product；
Real density：TD-1200, Bei Shide instrument Science and Technology Ltd. product；
Super constant temperature water tank：SC-15, Shanghai Shuan Shun industry developments Co., Ltd product；
Ash content：High-temperature electric resistance furnace SX2-2.5-12, Shanghai ray machine institute product；
Compacted density：TRCD-1, Mike Mo Ruitike（Shanghai）Instrument Ltd.'s product.
Assay method national standard：Compacted density GB1482-84；Real density GBT8330-2008；Specific surface area GB/
T19587-2004。
Half-cell test method is：Artificial graphite material, the N-Methyl pyrrolidone and 2% for containing 6 ~ 7% Kynoar
Conductive black by 91.6 ︰, 6.6 ︰ 1.8 mass ratio be uniformly mixed, be applied on copper foil, the pole piece coated, which is put into temperature, is
Be dried in vacuo in 110 DEG C of vacuum drying chambers 4 hours it is spare.Simulated battery be assemblied in the German Braun glove box of applying argon gas into
Row, the EC ︰ DEC ︰ DMC that electrolyte is 1M LiPF6 and volume ratio is 1 ︰, 1 ︰ 1, metal lithium sheet are to electrode, and chemical property is surveyed
Examination carries out on U.S. ArbinBT2000 type cell testers, charging/discharging voltage ranging from 0.005 to 1.0V, charge-discharge velocity
For 0.1C.
Be sieved method for testing performance：Sieve is converted into funnel-form, it is made to encase beaker mouth, rubber band is used in combination to be sleeved on beaker mouth
So that it is fixed, the slurry mixed is poured into a little sieve（200 mesh）On, it is gently squeezed with spoon, observation slurry sieving situation
How.If can not be sieved, the smaller sieve of mesh number is changed（If 100 mesh still can not be sieved, not re-sieving, then regarding tool
Body situation sees whether need to be coated with）, after choosing suitable sieve, slurry is poured on sieve, is gently squeezed with spoon, is slowly made
Slurry flows into following beaker, and sieve can be rinsed with water when needing to pay attention to oversize, then observes whether oversize has
Phenomena such as bulky grain.
The performance parameter of the artificial graphite material of 1 each embodiment of table
As can be seen from Table 1：Examples 1 and 2, by this method treated artificial plumbago negative pole material, compacted density
Respectively by 1.49g/cm3And 1.47g/cm3Promote 1.56g/cm3And 1.61g/cm3, capacity and efficiency is not affected, very
Density and volume average particle size D50 have reduction；Embodiment 3 and 4 adds by this method treated artificial plumbago negative pole material
Big fusion rotating speed can more improve compacted density, and raw material A is by 1.49g/cm3It is increased to 1.68g/cm3, raw material B is by 1.47g/cm3
It is increased to 1.74g/cm3；The lengthening processing time of embodiment 5 can more improve compacted density, by 1.47g/cm3It is increased to 1.80g/
cm3.From comparative example 1 it can be seen that changing the rotating speed of high speed mixer, the compacted density of raw material A does not change；From comparative example 2
It can be seen that changing the time of batch mixing, the compacted density of raw material B does not change；It can be seen that changing simultaneously mixed from comparative example 3
The batch mixing rotating speed and mixing time of material machine, the compacted density of material do not change.
The particle diameter distribution trend of the product of embodiment 2 before and after the processing distinguishes as depicted in figs. 1 and 2, the Electronic Speculum pattern of sample
As shown in Figure 3.The above results show that after the processing of the method for the present invention, tap density is significantly improved, and D50 has reduction,
It but keeps original size distribution trend, sample Electronic Speculum regular appearance, ash content not to increase, controls within the limits prescribed,
Treated negative material discharging efficiency and capacity are not affected, and the sieving performance of material is improved.
Claims (9)
1. a kind of preprocess method of artificial graphite material, which is characterized in that it includes the following steps：
(1) the D50 artificial graphite materials for being 16-22 μm are dried to moisture therein to percentage≤2% for accounting for material gross mass,
Dry artificial graphite material is obtained, the time of the drying is 1-3 hours；The temperature of the drying is 100-150 DEG C；
(2) artificial graphite material of the drying obtained by step (1) is modified in fusion machine in high speed with 1700-2200r/min's
Rotating speed batch mixing 3-30min is sieved later.
2. preprocess method as described in claim 1, which is characterized in that the D50 values of the artificial graphite material described in step (1)
It is 18-21 μm.
3. preprocess method as described in claim 1, which is characterized in that the single of the artificial graphite material described in step (1)
Treating capacity is 1.5-3kg.
4. preprocess method as described in claim 1, which is characterized in that the single of the artificial graphite material described in step (1)
Treating capacity is 2-2.5kg.
5. preprocess method as described in claim 1, which is characterized in that the time of the drying described in step (1) is that 1.5-3 is small
When；The temperature of the drying is 120-150 DEG C.
6. preprocess method as described in claim 1, which is characterized in that the batch mixing described in step (2) is with 1800-2000r/
The rotating speed batch mixing 10-20min of min.
7. preprocess method as described in claim 1, which is characterized in that the mesh number of step (2) described sieving is 200-250
Mesh.
8. the artificial graphite material as made from the preprocess method of claim 1~7 any one of them artificial graphite material.
9. application of the artificial graphite material as claimed in claim 8 in preparing cell negative electrode material.
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