CN103346294A - Preparation method of artificial graphite cathode material - Google Patents
Preparation method of artificial graphite cathode material Download PDFInfo
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- CN103346294A CN103346294A CN2013102543991A CN201310254399A CN103346294A CN 103346294 A CN103346294 A CN 103346294A CN 2013102543991 A CN2013102543991 A CN 2013102543991A CN 201310254399 A CN201310254399 A CN 201310254399A CN 103346294 A CN103346294 A CN 103346294A
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Abstract
The invention discloses a preparation method of an artificial graphite cathode material, and particularly relates to a preparation method of a clad lithium ion battery artificial graphite cathode material. The preparation method comprises the following steps: after reforming the artificial graphite by pulverization, cladding an ultramicropowder cladding material on the artificial graphite in a mechanical fusion machine, roasting, and graphitizing to obtain the artificial graphite cathode material with superior performance. The method is environment-friendly and can easily implement large-scale production; and the specific capacity per gram of the prepared lithium ion battery graphite cathode material exceeds 350 mAh/g, the initial Coulomb efficiency exceeds 94%, the tap density is greater than 1.1 g/cm<3>, and the specific area is less than 2 m<2>/g.
Description
Technical field
The present invention relates to a kind of method of lithium ion battery artificial plumbago negative pole material of coating.
Background technology
Artificial plumbago negative pole material cycle performance and good rate capability, good to the selectivity of electrolyte, be fit to be used as power lithium batteries such as electric automobile.
Common artificial plumbago negative pole material sells after adopting the nodularization system with the broken nodularization shaping of Delanium more.Mainly there is following problem in existing automatic spheroidization system: equipment is primarily aimed at the natural flake graphite nodularization and designs, the air-flow vortex ultra micro powder acc power that uses is the same, to artificial plumbago negative pole material nodularization shaping the time, the air-flow vortex ultra micro powder chance of equal-wattage causes the good particle of nodularization broken again, cause sphericity to be destroyed, yield reduces; In addition, in the nodularization later stage, the existing meticulous material of part is recovered, and the material that participates in nodularization significantly reduces, and still adopt the super pulverizing mill of high-power air-flow vortex to carry out nodularization this moment, can increase equipment energy consumption.
Still there are problems such as specific area is big, the gram specific capacity is low, compacted density is low in artificial plumbago negative pole material through the nodularization shaping.Be the better artificial plumbago negative pole material of processability, need that also it is carried out modification and handle.Patent CN101924209A handles needle coke by modifications such as catalyzed graphitization, coatings, make the artificial plumbago negative pole material of better performances; But its preparation raw material is needle coke, and price is expensive, and complicated process of preparation.Patent CN1691374A is coated on the Delanium surface with clad material after with dissolution with solvents, and the artificial plumbago negative pole material specific surface that makes is low, first the coulombic efficiency height; But introduce a large amount of solvents in the preparation process, complex process is big to environmental impact.Patent CN1649192A is crushed to back below the 2 μ m with hard pitch to be mixed with native graphite, and the natural graphite negative electrode material that makes coulombic efficiency first reaches 92%; But it only requires evenly to mix in preparation process, and it is poor slightly to cause covered effect to compare the liquid phase covered effect, and requires pitch is crushed to below the 2 μ m in preparation process, and existing micro mist equipment extremely difficulty reaches technological requirement.Therefore, how adopting more rational artificial plumbago negative pole material solid phase coating technology, is problem demanding prompt solution of present industry.
Summary of the invention
The objective of the invention is to avoid the deficiencies in the prior art that a kind of preparation method of artificial plumbago negative pole material is provided.The present invention coats evenly, technology is simple, cost is low, be convenient to large-scale production.
For realizing above purpose, the present invention is achieved through the following technical solutions: a kind of preparation method of artificial plumbago negative pole material, and its main feature is may further comprise the steps:
(1) granularity is broken less than the graphite of 4mm, with its nodularization, the graphite microparticles meso-position radius is 15~22 μ m after the nodularization, and specific area is less than 7m
2/ g, tap density is greater than 0.85g/cm
3
(2) the clad material asphalt powder is broken to meso-position radius 3~5 μ m;
(3) take by weighing graphite microparticles 80~95 weight portions of step (1), step (2) pitch micro mist 5~20 weight portions, place cone-type mixer slightly to mix blowing after at least 10 minutes, material after will slightly mixing again places in the mechanical fusion machine, start mechanical fusion machine afterwards, rotating speed with 500r/min~1000r/min merges 15~60min, makes pitch-coating at graphite surface, subsequently blowing;
(4) during the graphite powder that step (3) is coated with pitch is packed graphite crucible into, place ring-form calcining furnace to carry out roasting, the roasting maximum temperature is 1000 ℃~1400 ℃, is incubated 10~30 hours under maximum temperature;
(5) the graphite crucible of packing into of the graphite powder after the roasting of step (4), carry out graphitization at 2800 ℃~3200 ℃, namely make graphite cathode material.
The preparation method of described artificial plumbago negative pole material, the graphite described in the step (1) is broken to be that ultra-high power graphite electrode graphite is broken or ultra high power joint graphite is broken.The industry standard of ultra high power graphite electrode and ultra high power joint is YB/T4090-2000, refers to allow to use current density greater than 25A/cm
2Graphite electrode.
The preparation method of described artificial plumbago negative pole material, the pitch described in the step (2) is the high temperature modified coal tar pitch, its softening point is 100~140 ℃, coking value 〉=55%, toluene insolubles 〉=30%, ash content≤0.3%; Or mesophase pitch, its softening point is 250~290 ℃, coking value 〉=75%, toluene insolubles 〉=60%, ash content≤0.5%.
The preparation method of described artificial plumbago negative pole material, nodularization described in the step (1) is with its nodularization by multistage continuous balling device, described multistage continuous balling device includes by 2~8 of the super pulverizing mills of first group of air-flow vortex of order series connection by which is provided with the negative pressure of grader, pressure limit for-0.5MPa~-be linked in sequence 2~8 of 2~8 and the 3rd group super pulverizing mills of air-flow vortex of second group of super pulverizing mill of air-flow vortex of 1MPa air pipe, after the grader classification, be that the graphite microparticles of 22 μ m enters the fine particle collection device with meso-position radius, enter next stage or the super pulverizing mill of next group air-flow vortex greater than the graphite microparticles of 22 μ m.
The preparation method of described artificial plumbago negative pole material, first group of air-flow vortex ultra micro of described multistage continuous balling device powder acc power is 120~90kw; Second group of air-flow vortex ultra micro powder acc power is 90~70kw; The 3rd group of air-flow vortex ultra micro powder acc power is 70~30kw.
The present invention compared with prior art has following advantage:
1. adopt the broken and broken conduct coating of the superelevation joint graphite basis material of ultra high power graphite electrode, performance is good, and cost is low.
2. adopt the multistage continuous balling system of different capacity, under the prerequisite that guarantees the nodularization degree, improved yield, reduced energy consumption.
3. introduce the mechanical fusion device of chemical field as the coating equipment of negative material.In mechanical fusion device, constantly the be squeezed effect of power and shearing force of material, particle surface reaches a kind of mechanical molten condition under the effect of above-mentioned power, thereby the fine asphalt micro mist is coated on the micron-sized graphite granule, traditional relatively batch mixer can be realized coating more uniformly.
4. roasting process adopts industrial ring-form calcining furnace to carry out, and need not protective gas, and production capacity is big, and energy consumption is low.
5. the preparation method is simple, covered effect good, be convenient to large-scale production.
The present invention with the nodularization of the multistage continuous balling of the broken process of Delanium system after, realized that with micronized pitch more uniform solid phase coats in mechanical fusion device, obtained the silicon/carbon/graphite in lithium ion batteries negative material through roasting, graphitization again, its gram specific capacity surpasses 350mAh/g, coulombic efficiency surpasses 94% first, and tap density is greater than 1.1g/cm
3, specific area is less than 2m
2/ g.Silicon/carbon/graphite in lithium ion batteries negative material among the present invention also has the characteristics that cost is low, be easy to large-scale production.
Description of drawings
Fig. 1 looks schematic diagram for the master of the multistage continuous balling device of the present invention.
Among the figure: 1, first group first the super pulverizing mill of air-flow vortex; 2, grader; 3, induced draft pipeline; 4, first group of air-flow vortex ultra micro powder unit (being formed by 2~8 120~90kw air-flow vortex ultra micro powder machines); 5, second group first the super pulverizing mill of air-flow vortex; 6, second group of air-flow vortex ultra micro powder unit (being formed by 2~8 90~70kw air-flow vortex ultra micro powder machines); 7, the 3rd group first super pulverizing mill of air-flow vortex; 8, the 3rd group of air-flow vortex ultra micro powder unit (being formed by 2~8 70~30kw air-flow vortex ultra micro powder machines); 9, fine particle collection device.
Embodiment
The present invention is further described in conjunction with specific embodiments:
Embodiment 1: a kind of preparation method of artificial plumbago negative pole material may further comprise the steps:
(1) granularity is broken less than the graphite of 4mm, with its nodularization, the graphite microparticles meso-position radius is 15~22 μ m after the nodularization, and specific area is less than 7m
2/ g, tap density is greater than 0.85g/cm
3
(2) the clad material asphalt powder is broken to meso-position radius 3~5 μ m;
(3) take by weighing graphite microparticles 80~95 weight portions of step (1), step (2) pitch micro mist 5~20 weight portions, place cone-type mixer slightly to mix blowing after at least 10 minutes, material after will slightly mixing again places in the mechanical fusion machine, start mechanical fusion machine afterwards, rotating speed with 500r/min~1000r/min merges 15~60min, makes pitch-coating at graphite surface, subsequently blowing;
(4) during the graphite powder that step (3) is coated with pitch is packed graphite crucible into, place ring-form calcining furnace to carry out roasting, the roasting maximum temperature is 1000 ℃~1400 ℃, is incubated 10~30 hours under maximum temperature;
(5) the graphite crucible of packing into of the graphite powder after the roasting of step (4), carry out graphitization at 2800 ℃~3200 ℃, namely make graphite cathode material.
Graphite described in the step (1) is broken to be that ultra-high power graphite electrode graphite is broken or ultra high power joint graphite is broken.The industry standard of ultra high power graphite electrode and ultra high power joint is YB/T4090-2000, refers to allow to use current density greater than 25A/cm
2Graphite electrode.
Pitch described in the step (2) is the high temperature modified coal tar pitch, and its softening point is 100~140 ℃, coking value 〉=55%, toluene insolubles 〉=30%, ash content≤0.3%; Or mesophase pitch, its softening point is 250~290 ℃, coking value 〉=75%, toluene insolubles 〉=60%, ash content≤0.5%.
Embodiment 2:
Get granularity less than the ultra high power graphite electrode of 4mm broken (FangDa Carbon New Materials Science Co., Ltd), by by 2 of the super pulverizing mills of 120kw air-flow vortex, 4 of the super pulverizing mills of 90kw air-flow vortex, 4 nodularization systems that are composed in series of the super pulverizing mill of 70kw air-flow vortex with its nodularization, artificial graphite microparticles meso-position radius 15 μ m after the nodularization, specific area is 6.4m
2/ g, tap density 0.88g/cm
3, get artificial graphite microparticles 30kg after the nodularization.Then high temperature modified coal tar pitch (emerging Coal Chemical Industry Co., Ltd of Huanghua City SINONETS) is pulverized with airslide disintegrating mill (Weifang powder equipment Co., Ltd just far away), its meso-position radius 4.5 μ m get and pulverize back pitch micro mist 1.5kg.Place cone-type mixer (Wuxi celebrate prosperous powder equipment Co., Ltd) slightly to mix blowing after 10 minutes above-mentioned Delanium micro mist and pitch micro mist, material after will slightly mixing again places in the mechanical fusion machine (Wuxi celebrate prosperous powder equipment Co., Ltd), start mechanical fusion machine afterwards, rotating speed with 500r/min merges 30min, makes pitch-coating on the Delanium surface; The Delanium powder that will be coated with pitch is subsequently packed in the graphite crucible, places ring-form calcining furnace to carry out roasting, 1000 ℃ of roasting maximum temperatures, temperature retention time 30 hours; The graphite crucible of at last the Delanium powder after the roasting being packed into carries out graphitization at 2800 ℃~3200 ℃, namely makes artificial plumbago negative pole material.
Embodiment 3:
Get granularity less than the ultra high power graphite joint broken (FangDa Carbon New Materials Science Co., Ltd) of 4mm, by by 4 of the super pulverizing mills of 100kw air-flow vortex, 4 of the super pulverizing mills of 70kw air-flow vortex, 4 automatic spheroidization systems that are composed in series of the super pulverizing mill of 50kw air-flow vortex with its nodularization, artificial graphite microparticles meso-position radius 18 μ m after the nodularization, specific area is 5.6m
2/ g, tap density 0.90g/cm
3, get artificial graphite microparticles 30kg after the nodularization.Then mesophase pitch (FangDa Carbon New Materials Science Co., Ltd) is pulverized with airslide disintegrating mill (Weifang powder equipment Co., Ltd just far away), its meso-position radius 3.4 μ m get pitch micro mist 7.5kg.Place cone-type mixer (Wuxi celebrate prosperous powder equipment Co., Ltd) slightly to mix blowing after 10 minutes above-mentioned Delanium micro mist and pitch micro mist, material after will slightly mixing again places in the mechanical fusion machine (Wuxi celebrate prosperous powder equipment Co., Ltd), start mechanical fusion machine afterwards, rotating speed with 1000r/min merges 60min, makes pitch-coating on the Delanium surface; The Delanium powder that will be coated with pitch is subsequently packed in the graphite crucible, places ring-form calcining furnace to carry out roasting, 1400 ℃ of roasting maximum temperatures, temperature retention time 10 hours; The graphite crucible of at last the Delanium powder after the roasting being packed into carries out graphitization at 2800 ℃~3200 ℃, namely makes artificial plumbago negative pole material.
Embodiment 4:
Get granularity less than the ultra high power graphite joint broken (FangDa Carbon New Materials Science Co., Ltd) of 4mm, by by 4 of the super pulverizing mills of 90kw air-flow vortex, 8 of the super pulverizing mills of 70kw air-flow vortex, 8 automatic spheroidization systems that are composed in series of the super pulverizing mill of 30kw air-flow vortex with its nodularization, artificial graphite microparticles meso-position radius 22 μ m after the nodularization, specific area 4.3m
2/ g, tap density 0.95g/cm
3, get artificial graphite microparticles 30kg after the nodularization.Then mesophase pitch (FangDa Carbon New Materials Science Co., Ltd) is pulverized with airslide disintegrating mill (Weifang powder equipment Co., Ltd just far away), its meso-position radius 3.6 μ m get pitch micro mist 3.5kg.Place cone-type mixer (Wuxi celebrate prosperous powder equipment Co., Ltd) slightly to mix blowing after 10 minutes above-mentioned Delanium micro mist and pitch micro mist, material after will slightly mixing again places in the mechanical fusion machine (Wuxi celebrate prosperous powder equipment Co., Ltd), start mechanical fusion machine afterwards, rotating speed with 800r/min merges 15min, makes pitch-coating on the Delanium surface; The Delanium powder that will be coated with pitch is subsequently packed in the graphite crucible, places ring-form calcining furnace to carry out roasting, 1200 ℃ of roasting maximum temperatures, temperature retention time 20 hours; The graphite crucible of at last the Delanium powder after the roasting being packed into carries out graphitization at 2800 ℃~3200 ℃, namely makes artificial plumbago negative pole material.
Embodiment 5:
Described multistage continuous balling device include the super pulverizing mill 1 of first group of air-flow vortex by order series connection be 2~8 by which is provided with the negative pressure of grader 2, pressure limit for-0.5MPa~-the 1MPa air pipe second group of super pulverizing mill 5 of air-flow vortex that be linked in sequence is that 2~8 and the 3rd group of super pulverizing mill 7 of air-flow vortex are 2~8, after grader 2 classifications, be that the graphite microparticles of 22 μ m enters fine particle collection device 9 with meso-position radius, enter next stage or the super pulverizing mill of next group air-flow vortex greater than the graphite microparticles of 22 μ m.
Super pulverizing mill 1 power of first group of air-flow vortex of described multistage continuous balling device is 120~90kw; Second group of super pulverizing mill 5 power of air-flow vortex is 90~70kw; The 3rd group of super pulverizing mill 7 power of air-flow vortex are 70~30kw.
Experimental example:
The product of embodiment 2 to embodiment 4 is carried out electrochemical property test:
The performance of lithium ion battery negative material among check the present invention, adopt the half-cell method of testing, be specially: adopt graphite sample, the N-methyl pyrrolidone that contains 6~7% Kynoar and 2% conductive black among the present invention, mix, be applied on the Copper Foil, it is that 110 ℃ of vacuum drying chamber vacuumizes 4 hours are standby that the pole piece that coats is put into temperature.Simulated battery is assemblied in the German Braun glove box of applying argon gas and carries out, and electrolyte is 1MLiPF
6+ EC:DEC:DMC=1:1:1(volume ratio), metal lithium sheet is to electrode, and blue electronics (CT2001A type) cell tester carries out electrochemical property test in the Wuhan City, and the charging/discharging voltage scope is 0.005~1.0V, and charge-discharge velocity is 0.1C.
Each embodiment performance parameter is as shown in the table:
These parameters all meets the standard GB/T24533-2009 silicon/carbon/graphite in lithium ion batteries class negative material of lithium ion battery negative material.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. the preparation method of an artificial plumbago negative pole material is characterized in that may further comprise the steps:
(1) granularity is broken less than the graphite of 4mm, with its nodularization, the graphite microparticles meso-position radius is 15~22 μ m after the nodularization, and specific area is less than 7m
2/ g, tap density is greater than 0.85g/cm
3
(2) the clad material asphalt powder is broken to meso-position radius 3~5 μ m;
(3) take by weighing graphite microparticles 80~95 weight portions of step (1), step (2) pitch micro mist 5~20 weight portions, place cone-type mixer slightly to mix blowing after at least 10 minutes, material after will slightly mixing again places in the mechanical fusion machine, start mechanical fusion machine afterwards, rotating speed with 500r/min~1000r/min merges 15~60min, makes pitch-coating at graphite surface, subsequently blowing;
(4) during the graphite powder that step (3) is coated with pitch is packed graphite crucible into, place ring-form calcining furnace to carry out roasting, the roasting maximum temperature is 1000 ℃~1400 ℃, is incubated 10~30 hours under maximum temperature;
(5) the graphite crucible of packing into of the graphite powder after the roasting of step (4), carry out graphitization at 2800 ℃~3200 ℃, namely make graphite cathode material.
2. the preparation method of artificial plumbago negative pole material as claimed in claim 1, it is characterized in that: the graphite described in the step (1) is broken, and is broken or ultra high power joint graphite is broken for ultra-high power graphite electrode graphite.
3. the preparation method of artificial plumbago negative pole material as claimed in claim 1, it is characterized in that: the pitch described in the step (2) is the high temperature modified coal tar pitch, its softening point is 100~140 ℃, coking value 〉=55%, toluene insolubles 〉=30%, ash content≤0.3%; Or described pitch is mesophase pitch, and its softening point is 250~290 ℃, coking value 〉=75%, toluene insolubles 〉=60%, ash content≤0.5%.
4. the preparation method of artificial plumbago negative pole material as claimed in claim 1, it is characterized in that: the nodularization described in the step (1) for by multistage continuous balling device with its nodularization, described multistage continuous balling device includes by 2~8 of the super pulverizing mills of first group of air-flow vortex of order series connection by which is provided with the negative pressure of grader, pressure limit for-0.5MPa~-be linked in sequence 2~8 of 2~8 and the 3rd group super pulverizing mills of air-flow vortex of second group of super pulverizing mill of air-flow vortex of 1MPa air pipe, after the grader classification, be that the graphite microparticles of 22 μ m enters the fine particle collection device with meso-position radius, enter next stage or the super pulverizing mill of next group air-flow vortex greater than the graphite microparticles of 22 μ m.
5. the preparation method of artificial plumbago negative pole material as claimed in claim 3, it is characterized in that: first group of air-flow vortex ultra micro of described multistage continuous balling device powder acc power is 120~90kw; Second group of air-flow vortex ultra micro powder acc power is 90~70kw; The 3rd group of air-flow vortex ultra micro powder acc power is 70~30kw.
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CN106486653A (en) * | 2015-12-08 | 2017-03-08 | 宁波杉杉新材料科技有限公司 | A kind of liquid phase coating modified graphite cathode material and preparation method thereof |
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CN106898772A (en) * | 2017-03-17 | 2017-06-27 | 雅安乾润锂电池材料有限公司 | A kind of preparation method of high magnification high-pressure solid graphite cathode material |
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CN110203921A (en) * | 2019-06-13 | 2019-09-06 | 广东凯金新能源科技股份有限公司 | A kind of preparation method of lithium ion battery modified natural graphite |
CN112390252A (en) * | 2019-08-13 | 2021-02-23 | 贝特瑞新材料集团股份有限公司 | Cathode material based on carbon sundries, preparation method of cathode material and lithium ion battery |
CN112390252B (en) * | 2019-08-13 | 2024-04-12 | 贝特瑞新材料集团股份有限公司 | Carbon impurity-based negative electrode material, preparation method thereof and lithium ion battery |
CN111960413A (en) * | 2020-08-17 | 2020-11-20 | 内蒙古恒胜新能源科技有限公司 | Modification method of natural graphite negative electrode material |
CN112713264A (en) * | 2020-12-28 | 2021-04-27 | 宁波杉杉新材料科技有限公司 | Artificial graphite negative electrode material, preparation method, application and battery |
CN113964311A (en) * | 2021-11-23 | 2022-01-21 | 惠州亿纬锂能股份有限公司 | Graphite negative electrode material and preparation method and application thereof |
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