CN103879996A - Pretreatment method of artificial graphite material and obtained product and application - Google Patents
Pretreatment method of artificial graphite material and obtained product and application Download PDFInfo
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Abstract
The invention discloses a pretreatment method of an artificial graphite material, which is characterized by comprising the following steps: (1) drying an artificial graphite material with a D50 of 18-24 microns to reach a water percent of not more than 1% of the total mass of the material, so as to obtain a dry artificial graphite material; (2) mixing the dry artificial graphite material obtained in step (1) in a high-speed modification fusion machine with a rotating speed of 2300-2700 r/min for 5-15 min, and then sieving to obtain the product. The invention also provides an artificial graphite material prepared by the pretreatment method of an artificial graphite material, and an application in preparation of cell anode materials. The tap density of the artificial graphite material of the invention is significantly improved; the whole particle size distribution is not affected, and the distribution of large and small particles is more uniform; the regularity of the morphology is improved, the morphology is modified to be more complete and uniform, and the performance of capacity and efficiency is not affected; the properties are stable, and almost no difference exists between batches.
Description
Technical field
The present invention relates to a kind of pretreatment process and products obtained therefrom and application of synthetic graphite material.
Background technology
Along with the universalness of electronic installation, more and more desirability can better secondary cell.What attract people's attention especially is lithium ion battery, compared with NI-G or nickel metal hydride battery, uses lithium ion battery to have higher energy density, thereby has better use properties.Currently available technology has been carried out broad research for improving battery performance, but along with the further raising that battery performance is required, also needs to improve the tap density of battery, thereby improve on the whole the material property of synthetic graphite.
Synthetic graphite material has good processing use properties, but the low defect of ubiquity tap density.Synthetic graphite material is in process of manufacture, generally have the program of following process classification, and the production sequence of processing classification can have influence on the size-grade distribution of material, the processing wearing and tearing of machine can have influence on the granule-morphology of synthetic graphite, and then can make the tap density of material monolithic reduce.
In lithium ion battery design process, tap density is the quality of the measured unit volume after jolt ramming of the powder in container under prescribed condition.Lithium-ion-power cell is in making processes, and tap density has larger impact to battery performance.In general, tap density is larger, and the capacity of battery just can be accomplished higher, so tap density is also counted as one of reference index of material energy density.Tap density not only has relation with size, the density of particle, also and the pattern of particle have relation, what tap density was large generally has good particle normal distribution.Can think, under the certain condition of processing condition, tap density is larger, and the capacity of battery is higher.
In order to address the above problem, synthetic graphite generally will carry out follow-up surface modification treatment, to improve the tap density of material.The method that improves at present synthetic graphite tap density mainly contains the degree of graphitization that improves material, and the raising of degree of graphitization can make material softer, better press, thus the tap density of raising synthetic graphite.But the degree of graphitization that improves merely material can only make material softer, can't change the pattern of particle, the overall particle size of particle distributes and does not have large change, and therefore the raising degree of tap density is very limited.
Summary of the invention
Technical problem to be solved by this invention is that the particle surface correction imperfection in order to overcome existing synthetic graphite material and the subsequent disposal such as do not sieve cause the defect that tap density is not high, and provide a kind of powder tap density that improves synthetic graphite material, but do not affect the performance of the original size-grade distribution of material and capacity and efficiency, make the pattern regularity of material increase simultaneously, security is good, stable in properties, does not almost have pretreatment process and products obtained therefrom and the application of differentiated synthetic graphite material between batch.
One of technical scheme provided by the invention is: a kind of pretreatment process of synthetic graphite material, it comprises the steps:
(1) be per-cent≤1% that the synthetic graphite material of 18-24 μ m is dried to moisture wherein and accounts for material total mass by D50, obtain dry synthetic graphite material;
(2) by the dry synthetic graphite material of step (1) gained rotating speed batch mixing 5-15min with 2300-2700r/min in high speed modification fusion machine, sieve afterwards.
In the present invention, the described synthetic graphite material of step (1) is the various common artificial graphite raw material of this area routine; Preferably, the D50 value of described synthetic graphite material is 20-22 μ m.Described D50 is volume average particle size, corresponding particle diameter when the cumulative particle sizes percentile that refers to a sample reaches 50%, and its physical significance is that the particle that particle diameter is greater than it accounts for 50%, the particle that is less than it also accounts for 50%.
In the present invention, the single treatment amount of the described synthetic graphite material of step (1) is preferably 1.5-3kg, is more preferably 2-2.5kg, is 2.2kg best.
In the present invention, what step (1) was described is dried the drying operation for this area routine, generally in loft drier, carries out; The described dry time is preferably 1-3 hour, is more preferably 1.5-3 hour; Described dry temperature is preferably 100-140 DEG C, is more preferably 120-140 DEG C, is best 140 DEG C.
In the present invention, the described batch mixing of step (2) is preferably the rotating speed batch mixing 5-10min with 2300-2500r/min.Before described batch mixing, preferably also comprise the machine of batch mixing is cleared up, detected, there is no other impurity as good.
In the present invention, the order number sieving described in step (2) is preferably 200-250 order, is more preferably 250 orders, to remove impurity and macrobead.
In the present invention, after sieving step (2) Suo Shu, the synthetic graphite material of gained before reality is used, preferably also step censorship processing routinely.
Two of technical scheme provided by the invention is: the synthetic graphite material that the pretreatment process of foregoing synthetic graphite material makes.
Three of technical scheme provided by the invention is: the synthetic graphite material that the pretreatment process of foregoing synthetic graphite material makes is in the application of preparing in cell negative electrode material.
In the present invention, described cell negative electrode material is preferably lithium ion battery negative material.
Meeting on the basis of this area general knowledge, above-mentioned each optimum condition, can arbitrary combination, obtains the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material be commercially available obtaining all.
Positive progressive effect of the present invention is: the tap density of synthetic graphite material of the present invention obviously improves; Overall particle size distributes can be not influenced, and size particles distributes more evenly; Pattern regularity increases, and modifies more complete evenly, does not affect the performance of capacity and efficiency; Stable in properties, does not almost have difference between batch.The pretreatment process simple possible of synthetic graphite material of the present invention, is applicable to suitability for industrialized production.
Brief description of the drawings
Fig. 1 is embodiment 2 raw meal particle size distribution plan before treatment.
Fig. 2 is embodiment 2 raw meal particle size distribution plan after treatment.
Fig. 3 is the material Electronic Speculum figure before and after embodiment 2 processes, and wherein, (a) is embodiment 2 material Electronic Speculum before treatment figure; (b) be embodiment 2 material Electronic Speculum after treatment figure.
Embodiment
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, according to ordinary method and condition, or selects according to catalogue.
The synthetic graphite series products that the synthetic graphite material using in following embodiment is produced for Shanghai Shanshan Science and Technology Co., Ltd.
Synthetic graphite material (being designated as raw material A), the D50 of commodity mark is 20 μ m left and right, and raw material is 2.2kg altogether, and the volume average particle size D50 that sample detects before processing is 20.6 μ m, and true density is 2.24g/cm
3, tap density is 0.80g/cm
3.
(1) synthetic graphite material is put into loft drier, through 120 DEG C of drying treatment 1.5 hours, account for per-cent≤1% of material total mass to moisture;
(2) whether the equipment operation of inspection fusion machine is normal, and cleaning fusion machine, guarantees inclusion-free; Be that 20.6 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2kg D50, the time is 5 minutes, rotating speed 2300r/m; The material processing of sieving afterwards, crosses grit number 250 orders.
After testing, material particle diameter is after treatment 20.4 μ m, and true density is 2.24g/cm
3, tap density is 0.85g/cm
3.
Embodiment 2
Synthetic graphite material (being designated as raw material B), the D50 of commodity mark is 22 μ m left and right, and raw material is 1.5kg altogether, and the volume average particle size D50 that sample detects before processing is 22.8 μ m, true density 2.24g/cm
3, tap density is 0.82g/cm
3.
(1) synthetic graphite material is put into loft drier, through 140 DEG C of drying treatment 1.0 hours, account for per-cent≤1% of material total mass to moisture;
(2) whether the equipment operation of inspection fusion machine is normal, and cleaning mixer, guarantees inclusion-free; Be that 22.8 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2.5kg D50, the time is 5 minutes, rotating speed 2300r/m; The material processing of sieving afterwards, crosses grit number 250 orders.
After testing, material particle diameter is after treatment 22.6 μ m, and true density is 2.24g/cm
3, tap density is 0.88g/cm
3.
Embodiment 3
Synthetic graphite material (being designated as raw material A), the D50 of commodity mark is 20 μ m left and right, and raw material is 2.2kg altogether, and the volume average particle size D50 that sample detects before processing is 20.6 μ m, true density 2.24g/cm
3, tap density 0.80g/cm
3.
(1) synthetic graphite material is put into loft drier, through 100 DEG C of drying treatment 3.0 hours, account for per-cent≤1% of material total mass to moisture;
(2) whether the equipment operation of inspection fusion machine is normal, and cleaning fusion machine, guarantees inclusion-free; Be that 20.6 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2kg D50, the time is 10 minutes, rotating speed 2300r/m; The material processing of sieving afterwards, crossing grit number is 250 orders.
After testing, material particle diameter is after treatment 20.3 μ m, and true density is 2.24g/cm
3, tap density is 0.88g/cm
3.
Embodiment 4
Synthetic graphite material (being designated as raw material B), the D50 of commodity mark is 22 μ m left and right, and raw material is 3kg altogether, and the volume average particle size D50 that sample detects before processing is 22.8 μ m, true density 2.24g/cm
3, tap density 0.82g/cm
3.
(1) synthetic graphite material is put into loft drier, through 120 DEG C of drying treatment 1.5 hours, account for per-cent≤1% of material total mass to moisture, make material monolithic be dry finely powdered;
(2) whether the equipment operation of inspection mixer is normal, and cleaning mixer, guarantees inclusion-free; Be that 22.8 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2.2kg D50, the time is 5 minutes, rotating speed 2500r/m; The material processing of sieving afterwards, crossing grit number is 250 orders.
After testing, material particle diameter is after treatment 22.2 μ m, and true density is 2.24g/cm
3, tap density is 0.91g/cm
3.
Synthetic graphite material (being designated as raw material B), the D50 of commodity mark is 22 μ m left and right, and raw material is 2kg altogether, and the volume average particle size D50 that sample detects before processing is 22.8 μ m, true density 2.24g/cm
3, tap density 0.82g/cm
3.
(1) synthetic graphite material is put into loft drier, through 130 DEG C of drying treatment 1.5 hours, account for per-cent≤1% of material total mass to moisture, make material monolithic be dry finely powdered;
(2) equipment that checks fusion machine moves, and guarantees normally, and cleaning fusion machine, guarantees inclusion-free; Be that 22.8 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2.2kg D50, the time is 15 minutes, rotating speed 2700r/m; The material processing of sieving afterwards, crossing grit number is 200 orders.
After testing, material particle diameter is after treatment 22.2 μ m, and true density is 2.24g/cm
3, tap density is 0.95g/cm
3.
Synthetic graphite material (being designated as raw material A), the D50 of commodity mark is 18 μ m left and right, and raw material is 2.5kg altogether, and the volume average particle size D50 that sample detects before processing is 18.2 μ m, and true density is 2.24g/cm
3, tap density is 0.81g/cm
3.
(1) synthetic graphite material is put into loft drier, through 120 DEG C of drying treatment 1.5 hours, account for per-cent≤1% of material total mass to moisture;
(2) whether the equipment operation of inspection fusion machine is normal, and cleaning fusion machine, guarantees inclusion-free; Be that 18.0 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2kg D50, the time is 11 minutes, rotating speed 2500r/m; The material processing of sieving afterwards, crosses grit number 250 orders.
After testing, material particle diameter is after treatment 17.9 μ m, and true density is 2.24g/cm
3, tap density is 0.84g/cm
3.
Synthetic graphite material (being designated as raw material B), the D50 of commodity mark is 24 μ m left and right, and raw material is 2.2kg altogether, and the volume average particle size D50 that sample detects before processing is 24.8 μ m, true density 2.24g/cm
3, tap density 0.83g/cm
3.
(1) synthetic graphite material is put into loft drier, through 130 DEG C of drying treatment 1.5 hours, account for per-cent≤1% of material total mass to moisture, make material monolithic be dry finely powdered;
(2) equipment that checks fusion machine moves, and guarantees normally, and cleaning fusion machine, guarantees inclusion-free; Be that 24.8 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2.2kg D50, the time is 11 minutes, rotating speed 2700r/m; The material processing of sieving afterwards, crossing grit number is 250 orders.
After testing, material particle diameter is after treatment 22.2 μ m, and true density is 2.24g/cm
3, tap density is 0.91g/cm
3.
Comparative example 1
Synthetic graphite material (being designated as raw material A), the D50 of commodity mark is 20 μ m left and right, and raw material is 2kg altogether, and the volume average particle size D50 that sample detects before processing is 20.6 μ m, true density 2.24g/cm
3, tap density 0.80g/cm
3.
(1) synthetic graphite material is put into loft drier, through 140 DEG C of drying treatment 1.5 hours;
(2) whether the equipment operation of inspection fusion machine is normal, and cleaning fusion machine, guarantees inclusion-free; Be that 20.6 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2.2kg D50, the time is 3 minutes, rotating speed 2300r/m; The material processing of sieving afterwards, crossing grit number is 250 orders.
After testing, material particle diameter is after treatment 20.6 μ m, and true density is 2.24g/cm
3, tap density is 0.80g/cm
3.
Comparative example 2
Synthetic graphite material (being designated as raw material B), the D50 of commodity mark is 22 μ m left and right, and raw material is 2.2kg altogether, and the volume average particle size D50 that sample detects before processing is 22.8 μ m, true density 2.24g/cm
3, tap density 0.82g/cm
3.
(1) synthetic graphite material is put into loft drier, through 120 DEG C of drying treatment 1.5 hours;
(2) whether the equipment operation of inspection fusion machine is normal, and cleaning mixer, guarantees inclusion-free; Be that 22.8 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2.2kg D50, the time is 15 minutes, rotating speed 1000r/m; The material processing of sieving afterwards.
After testing, material particle diameter is after treatment 22.8 μ m, and true density is 2.24g/cm
3, tap density is 0.82g/cm
3.
Comparative example 3
Synthetic graphite material (being designated as raw material B), the D50 of commodity mark is 22 μ m left and right, and raw material is 2.2kg altogether, and the volume average particle size D50 that sample detects before processing is 22.8 μ m, true density 2.24g/cm
3, tap density 0.82g/cm
3.
(1) synthetic graphite material is put into loft drier, through 120 DEG C of drying treatment 1.5 hours;
(2) whether the equipment operation of inspection fusion machine is normal, and cleaning mixer, guarantees inclusion-free; Be that 22.8 μ m synthetic graphite materials are put into high speed modification fusion machine batch mixing by 2.2kg D50, the time is 3 minutes, rotating speed 1000r/m; The material processing of sieving afterwards, crossing grit number is 250 orders.
After testing, material particle diameter is after treatment 22.8 μ m, and true density is 2.24g/cm
3, tap density is 0.82g/cm
3.
Effect embodiment
Artificial plumbago negative pole material in embodiment 1 ~ 7 is carried out respectively to particle diameter, true density, a tap density and ash index test that grades; Adopt half-cell testing method the synthetic graphite material in embodiment 1 ~ 7 to be carried out to the test of loading capacity and first charge-discharge efficiency, result is all listed in table 1.The Performance Detection of simultaneously also sieving, result is all listed in table 2.
Instrument title and model that test is used are as follows:
Laser fineness gage: MS2000, Dandong Bai Te Instrument Ltd. product;
True density: TD-1200, Bei Shide instrument Science and Technology Ltd. product;
Super constant temperature water tank: SC-15, Shanghai Shuan Shun industry development company limited product;
Ash content: high-temperature electric resistance furnace SX2-2.5-12, Shanghai ray machine institute product;
Tap density: TRMD-1, Mike Mo Ruitike (Shanghai) Instrument Ltd. product.
Measuring method national standard: tap density GB/T5162-2006/ISO3953:1993; True density GBT8330-2008; Specific surface area GB/T19587-2004.
Half-cell testing method is: synthetic graphite material, the N-Methyl pyrrolidone that contains 6 ~ 7% polyvinylidene difluoride (PVDF) and 2% graphitized carbon black mix by the mass ratio of 91.6 ︰ 6.6 ︰ 1.8, be applied on Copper Foil, it is that 110 DEG C of vacuum drying oven vacuum-dryings 4 hours are for subsequent use that the pole piece coating is put into temperature.Simulated battery is assemblied in the German Braun glove box of applying argon gas and carries out, electrolytic solution is that 1M LiPF6 and volume ratio are the EC ︰ DEC ︰ DMC of 1 ︰ 1 ︰ 1, metal lithium sheet is to electrode, electrochemical property test carries out on U.S. ArbinBT2000 type cell tester, charging/discharging voltage scope is 0.005 to 1.0V, and charge-discharge velocity is 0.1C.
Method for testing performance sieves: screen cloth is converted into funnel-form, makes it encase beaker mouth, and be enclosed within beaker mouth with bungee it is fixed, pour the slurry mixing into a little screen cloth (200 order) upper, push gently with spoon, observe the slurry what state of sieving.If cannot sieve, change the screen cloth that order number is less (if 100 orders still cannot sieve, no longer sieve, see whether need coating depending on particular case again), choose after suitable screen cloth, slurry is poured on screen cloth, push gently with spoon, whether slowly make slurry flow into beaker below, in the time should be noted that screen overflow, can rinse screen cloth for water, then observing screen overflow has the phenomenons such as macrobead.
The performance perameter of the synthetic graphite material of the each embodiment of table 1
As can be seen from Table 1: embodiment 1 and 2, through present method artificial plumbago negative pole material after treatment, tap density is respectively by 0.80g/cm
3and 0.82g/cm
3rise to 0.85g/cm
3and 0.88g/cm
3, true density, capacity and efficiency are not affected, and volume average particle size D50 has reduction; Embodiment 3 and 4, through present method artificial plumbago negative pole material after treatment, strengthens fusion rotating speed and can more improve tap density, and raw material A is by 0.80g/cm
3bring up to 0.88g/cm
3, raw material B is by 0.82g/cm
3bring up to 0.89g/cm3; Embodiment 5 lengthens the treatment time and can more improve tap density, by 0.82g/cm
3bring up to 0.95g/cm
3.Comparative example 1～3 changes fusion machine rotating speed and changes all can have bad impact to the powder tap density that improves synthetic graphite process period.
Respectively as depicted in figs. 1 and 2, the Electronic Speculum pattern of sample as shown in Figure 3 for the size distribution trend of the product before and after embodiment 2 processes.The above results shows, after method of the present invention is processed, the tap density of synthetic graphite material is significantly improved, D50 has reduction, but keeps original size-grade distribution trend, and sample Electronic Speculum pattern is regular, ash content does not increase, control within the limits prescribed, negative material discharging efficiency after treatment and capacity are not affected, and the performance of sieving of material is improved.
Claims (10)
1. a pretreatment process for synthetic graphite material, is characterized in that, it comprises the steps:
(1) be per-cent≤1% that the synthetic graphite material of 18-24 μ m is dried to moisture wherein and accounts for material total mass by D50, obtain dry synthetic graphite material;
(2) by the dry synthetic graphite material of step (1) gained rotating speed batch mixing 5-15min with 2300-2700r/min in high speed modification fusion machine, sieve afterwards.
2. pretreatment process as claimed in claim 1, is characterized in that, the D50 value of the described synthetic graphite material of step (1) is 20-22 μ m.
3. pretreatment process as claimed in claim 1, is characterized in that, the single treatment amount of the described synthetic graphite material of step (1) is 1.5-3kg.
4. pretreatment process as claimed in claim 1, is characterized in that, the single treatment amount of the described synthetic graphite material of step (1) is 2-2.5kg.
5. pretreatment process as claimed in claim 1, is characterized in that, the described dry time of step (1) is 1-3 hour; Described dry temperature is 100-140 DEG C.
6. pretreatment process as claimed in claim 1, is characterized in that, the described dry time of step (1) is 1.5-3 hour; Described dry temperature is 120-140 DEG C.
7. pretreatment process as claimed in claim 1, is characterized in that, the described batch mixing of step (2) is the rotating speed batch mixing 5-10min with 2300-2500r/min.
8. pretreatment process as claimed in claim 1, is characterized in that, the order number sieving described in step (2) is 200-250 order.
9. the synthetic graphite material that the pretreatment process of the synthetic graphite material as described in claim 1～8 any one makes.
10. synthetic graphite material as claimed in claim 9 is in the application of preparing in cell negative electrode material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106477569A (en) * | 2015-12-08 | 2017-03-08 | 宁波杉杉新材料科技有限公司 | A kind of preprocess method of artificial graphite material and products obtained therefrom and application |
| CN107871854A (en) * | 2016-09-27 | 2018-04-03 | 宁波杉杉新材料科技有限公司 | A kind of preparation method of graphite negative material of lithium ion battery second particle |
| CN109273713A (en) * | 2018-08-22 | 2019-01-25 | 广东东岛新能源股份有限公司 | A kind of power battery cathode shaping char particle and preparation method thereof |
| CN113023721A (en) * | 2021-02-09 | 2021-06-25 | 广东东岛新能源股份有限公司 | High-tap spherical graphite and preparation method and application thereof |
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2012
- 2012-12-21 CN CN201210563262.XA patent/CN103879996A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106477569A (en) * | 2015-12-08 | 2017-03-08 | 宁波杉杉新材料科技有限公司 | A kind of preprocess method of artificial graphite material and products obtained therefrom and application |
| CN107871854A (en) * | 2016-09-27 | 2018-04-03 | 宁波杉杉新材料科技有限公司 | A kind of preparation method of graphite negative material of lithium ion battery second particle |
| CN109273713A (en) * | 2018-08-22 | 2019-01-25 | 广东东岛新能源股份有限公司 | A kind of power battery cathode shaping char particle and preparation method thereof |
| CN113023721A (en) * | 2021-02-09 | 2021-06-25 | 广东东岛新能源股份有限公司 | High-tap spherical graphite and preparation method and application thereof |
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Application publication date: 20140625 |