CN101367518A - Method for preparing natural spherical plumbago with circular reshaping classification - Google Patents
Method for preparing natural spherical plumbago with circular reshaping classification Download PDFInfo
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- CN101367518A CN101367518A CNA2008101572816A CN200810157281A CN101367518A CN 101367518 A CN101367518 A CN 101367518A CN A2008101572816 A CNA2008101572816 A CN A2008101572816A CN 200810157281 A CN200810157281 A CN 200810157281A CN 101367518 A CN101367518 A CN 101367518A
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Abstract
The invention relates to a method for preparing the graphite powder, in particular relates to a method for preparing the graphite powder that is applied to the cathode of the lithium-ion secondary battery, which aims at overcoming the weaknesses of the prior natural spherical graphite powder preparation method that the craftwork is complicated, the quality of the obtained product is uniform and the production efficiency is low, so that a method for preparing the natural spherical graphite in the cycling shaping classification way. The natural crystalline flake graphite is primarily crashed in a mechanical crashing machine, and is cycled for milling, shaping and classification in a plurality of shaping classification machines. The method has simple craftwork and high control precision of the classification; the quality of the prepared natural spherical graphite powder is stable; the foreign matters in the graphite can be thoroughly removed; the content of the fixed carbon is high; at the same time, the production efficiency is improved, and the method is free from polluting the production environment.
Description
Technical field
The present invention relates to a kind of Graphite Powder 99 preparation method, especially the preparation method of the Graphite Powder 99 of lithium ion secondary battery negative pole use.
Background technology
Along with the anxiety of global energy, energy-saving lithium cell industry has obtained unprecedented development, and the battery that various power consumptions are big is replaced by lithium cell gradually.Lithium-ion secondary cell is good with its voltage height, safety performance, memory-less effect, have extended cycle life and advantage such as non-environmental-pollution and obtain widespread use.Development along with portable electric product, people are more and more higher to the requirement of used battery wherein, be presented as that mainly volume is little, the electricity consumption time long, the good and long service life of two-forty charge-discharge performance, especially nearly electric bicycle of greatly developing in 2 years, electromobile and the common required power cell of power tool require very high to the two-forty charge-discharge performance.
Graphite is negative material the most frequently used in the lithium-ion secondary cell, and wherein natural spherical plumbago is because its good electrical conductivity, cycle index is many, reversible capacity is big, energy is good, low cost and other advantages, has replaced synthetic graphite in the past gradually.When the specification requirement of control natural spherical plumbago, method commonly used at present has the screening sieve method, this method complex process, and the Quality Control Links leak is more, and precision is low; The shaping grading machine has also obtained application gradually in the preparation natural spherical plumbago in addition, but preparation technology commonly used at present adopts the unit preparation, the problem that adopts separate unit shaping grading machine to exist is: when product requirement is thin, need carry out the shaping classification to graphite to this, therefore when the shaping grading machine lead to go over the shaping classification after, the Graphite Powder 99 that makes need be collected again, feed intake once more and carry out the shaping classification, the time that at every turn feeds intake needs about 1 hour, if shaping classification 10 times, only feeding intake just needs about 10 hours time, has also expended great amount of manpower and material simultaneously, reduce production efficiency, and caused dust pollution easily in the process that feeds intake.
Summary of the invention
The quality product that the objective of the invention is to overcome preparation method's complex process of existing natural spherical plumbago powder and make is inhomogeneous, one-tenth produces inefficient defective, a kind of method of utilizing preparing natural spherical plumbago with circular reshaping classification has been proposed, its technology is simple, stepped control precision height, the natural spherical plumbago opaque amount that makes is stable, removes impurity wherein more up hill and dale, fixedly the carbon content height, improved production efficiency simultaneously, can not pollute production environment.
The present invention adopts following technical scheme to realize: a kind of method of preparing natural spherical plumbago with circular reshaping classification, and this method may further comprise the steps:
(1) be that 80 order to 200 purpose natural flake graphites are put into mechanical crusher and carried out elementary pulverizing with granularity, the pulverizing time is 30 minutes to 1 hour, and the median size that makes the graphite granule after the pulverizing is between 10um-80um;
(2) graphite after the pulverizing is directly linked in the shaping grading machine through pipeline, graphite granule is ground, detect by the graphite granule of proofing unit after the nodularization shaping, adjusting frequency conversion makes ultra-fine grain enter the full blast loading head, to meet the requirements is that particle diameter is at 10um-80um, be shaped as sphere or native bean-shaped natural spherical plumbago particle is collected by tornado feeder set, and discharge by star-like smooth wind device;
(3) the undesirable product after first shaping grading machine shaping classification is linked by pipeline in second shaping grading machine, carry out nodularization again and grind shaping, detect classification by proofing unit after the shaping, qualified product is collected, underproof product is linked next shaping grading machine, promptly the shaping classification is carried out in circulation successively, until qualified;
(4) by above-mentioned circular grinding shaping 6-8 hours, utilize the proofing unit classification, superfine and fines segregation in irregular shape are gone out, and collect satisfactory natural spherical plumbago;
(5) adopt ultrasonic wave to satisfactory natural spherical plumbago separating impurity.
Among the present invention, described shaping grading machine is horizontal grading machine or air-flow vortex pulverizing mill, need 8-20 shaping grading machines in the circular reshaping classification process, according to the proofing unit that uses in the shaping classification process detected results such as the particle diameter of graphite granule, shape are determined in the actual production.The particle diameter of qualified graphite granule should be between 10um-80um, and its shape should be sphere or potato shape.
Above-mentioned proofing unit comprises laser particle analyzer, microscopic imaging apparatus, density instrument and specific surface area instrument, wherein laser particle analyzer, microscopic imaging apparatus and specific surface area instrument are respectively applied for particle diameter, shape and the surface-area of measuring graphite granule, and the density instrument is used to detect the tap density of natural spherical plumbago powder.In the shaping classification process, by the strict control of above-mentioned test set natural spherical plumbago particulate granularity, shape etc., satisfactory graphite granule to be collected, not satisfactory particle is proceeded the shaping classification, guaranteed the quality of natural spherical plumbago, and quality stability is better.
Graphite Powder 99 after the shaping classification has further improved the purity and the quality stability of natural spherical plumbago powder by the ultrasonic wave separating impurity.
The invention has the beneficial effects as follows: pass through preparing natural spherical plumbago with circular reshaping classification, and in the shaping classification, graphite granule is detected by proofing unit, quality product has been carried out strict control, the control accuracy height, improved the degree of compactness of product, improved natural spherical plumbago particulate distribute spacing and face value, quality stability is better, and fixedly carbon content can reach 99.93%-99.995%; The natural spherical plumbago powder that makes is carried out the ultrasonic wave removal of impurities, improved the purity of natural spherical plumbago powder; In addition, compare with separate unit shaping grading machine, uniting many shaping grading machines carries out circular reshaping to graphite and has saved the time that repeatedly feeds intake, required manpower and materials have also been reduced simultaneously, separate unit shaping grading machine needs many people to safeguard, and after adopting many shaping grading machines, a people can safeguard many shaping grading machines simultaneously, the per capital production of separate unit shaping grading machine can only reach 300kg, and the per capital production after this employing present method can be up to 2000kg, production efficiency improves greatly, and can not produce dust pollution.
Embodiment
Embodiment 1
Utilizing method of the present invention to prepare specification is that the step of 0.98 natural spherical plumbago is as follows for 20um, tap density for D50, granularity:
At first, the natural flake graphite of granularity between 80 order to 200 orders carried out 30 minutes-1 hour elementary pulverizing in mechanical crusher, the median size that makes the graphite granule after the pulverizing is between 10um-80um.
Graphite granule after the elementary pulverizing is directly linked in the air-flow vortex pulverizing mill by pipeline: at first graphite granule is carried out nodularization and grind shaping in the air-flow vortex pulverizing mill, and then carry out classification.During classification, utilize laser particle analyzer, microscopic imaging apparatus, density instrument and specific surface area instrument to detect granularity, shape, tap density and the surface-area of graphite granule respectively, make ultra-fine grain enter the full blast loading head by adjusting frequency conversion, with satisfactory natural spherical plumbago, be that particle diameter is, is shaped as sphere or potato shape, tap density to be that 0.98 spherical graphite particle is collected by tornado feeder set between the 20um, and discharge by star-like smooth wind device; Underproof graphite granule is linked in next air-flow vortex pulverizing mill by pipeline in the testing process, through nodularization shaping and detection classification, qualified graphite granule is collected again, and underproof product is linked in next air-flow vortex pulverizing mill again.Carry out above-mentioned following and grind shaping and classification after 6-8 hours, satisfactory graphite granule is collected.The platform number of the air-flow vortex pulverizing mill that is adopted in present method is 8.In addition, except can adopting the air-flow vortex pulverizing mill, can also adopt other shaping grading machines.
In above-mentioned circular reshaping classification process, 2 technician of general only needs can finish the maintenance service to 8 shaping grading machines.Wherein separate unit output is 750kg, and per capital production can reach 2500kg, has improved production efficiency greatly.
At last, the above-mentioned natural spherical plumbago powder separating impurity that utilizes ultrasonic wave to collect further improves the fixedly carbon content and the quality of natural spherical plumbago.The fixedly carbon content of the natural spherical plumbago that makes through this method is between 99.93%-99.995%, and quality stability is better.
Spherical graphite by this method preparation is the finished product that comes from same system, so the quality stable homogeneous, the proofing unit by the advanced person in the shaping classification detects, and by the circular grinding shaping, has improved the control accuracy of finished product.
Embodiment 2
Utilizing method of the present invention to prepare specification is that the step of 1.02 natural spherical plumbago is as follows for 17um, tap density for D50, granularity:
At first, the natural flake graphite of granularity between 80 order to 200 orders carried out 30 minutes-1 hour elementary pulverizing in mechanical crusher, the median size that makes the graphite granule after the pulverizing is between 10um-80um.
Graphite granule after the elementary pulverizing is directly linked in the air-flow vortex pulverizing mill by pipeline: at first graphite granule is carried out nodularization and grind shaping in the air-flow vortex pulverizing mill, and then carry out classification.During classification, utilize laser particle analyzer, microscopic imaging apparatus, density instrument and specific surface area instrument to detect granularity, shape, tap density and the surface-area of graphite granule respectively, make ultra-fine grain enter the full blast loading head by adjusting frequency conversion, with satisfactory natural spherical plumbago, be that particle diameter is 17um, to be shaped as sphere or potato shape, tap density be that 0.98 spherical graphite particle is collected by tornado feeder set, and discharge by star-like smooth wind device; Underproof graphite granule is linked in next air-flow vortex pulverizing mill by pipeline in the testing process, through nodularization shaping and detection classification, qualified graphite granule is collected again, and underproof product is linked in next air-flow vortex pulverizing mill again.Carry out above-mentioned following and grind shaping and classification after 6-8 hours, satisfactory graphite granule is collected.The platform number of the air-flow vortex pulverizing mill that is adopted in present method is 10.In addition, except can adopting the air-flow vortex pulverizing mill, can also adopt other shaping grading machines.
In the circular reshaping classification process, generally need 3 technician to finish maintenance service to 10 shaping grading machines.Wherein separate unit output is 600kg, and per capital production can reach 1800kg.
At last, the above-mentioned natural spherical plumbago powder separating impurity that utilizes ultrasonic wave to collect further improves the fixedly carbon content and the quality of natural spherical plumbago.The fixedly carbon content of the natural spherical plumbago that makes through this method is between 99.93%-99.995%, and quality stability is better.
Other are with embodiment 1.
Embodiment 3
Utilizing method of the present invention to prepare specification is that the step of 1.02 natural spherical plumbago is as follows for 12um, tap density for D50, granularity:
At first, the natural flake graphite of granularity between 80 order to 200 orders carried out 30 minutes-1 hour elementary pulverizing in mechanical crusher, the median size that makes the graphite granule after the pulverizing is between 10um-80um.
Graphite granule after the elementary pulverizing is directly linked in the air-flow vortex pulverizing mill by pipeline: at first graphite granule is carried out nodularization and grind shaping in the air-flow vortex pulverizing mill, and then carry out classification.During classification, utilize laser particle analyzer, microscopic imaging apparatus, density instrument and specific surface area instrument to detect granularity, shape, tap density and the surface-area of graphite granule respectively, make ultra-fine grain enter the full blast loading head by adjusting frequency conversion, with satisfactory natural spherical plumbago, be that particle diameter is 12um, to be shaped as sphere or potato shape, tap density be that 0.98 spherical graphite particle is collected by tornado feeder set, and discharge by star-like smooth wind device; Underproof graphite granule is linked in next air-flow vortex pulverizing mill by pipeline in the testing process, through nodularization shaping and detection classification, qualified graphite granule is collected again, and underproof product is linked in next air-flow vortex pulverizing mill again.Carry out above-mentioned following and grind shaping and classification after 6-8 hours, satisfactory graphite granule is collected.The platform number of the air-flow vortex pulverizing mill that is adopted in present method is 20.In addition, except can adopting the air-flow vortex pulverizing mill, can also adopt other shaping grading machines.
Because the platform number of shaping grading machine is more,, generally need 4 technician to finish maintenance service to 20 shaping grading machines in order to guarantee the total system works better.Wherein separate unit output is 300kg, and per capital production can reach 600kg.
At last, the above-mentioned natural spherical plumbago powder separating impurity that utilizes ultrasonic wave to collect further improves the fixedly carbon content and the quality of natural spherical plumbago.The fixedly carbon content of the natural spherical plumbago that makes through this method is between 99.93%-99.995%, and quality stability is better.
Other are with embodiment 1.
Claims (4)
1. the method for a preparing natural spherical plumbago with circular reshaping classification is characterized in that this method may further comprise the steps:
(1) be that 80 order to 200 purpose natural flake graphites are put into mechanical crusher and carried out elementary pulverizing with granularity, the pulverizing time is 30 minutes to 1 hour, and the median size of the graphite granule after the pulverizing is between 10um-80um;
(2) graphite after the pulverizing is directly linked in the shaping grading machine through pipeline, graphite granule is ground, detect by the graphite granule of proofing unit after the nodularization shaping, adjusting frequency conversion makes ultra-fine grain enter the full blast loading head, to meet the requirements is that particle diameter is at 10um-80um, be shaped as sphere or native bean-shaped natural spherical plumbago particle is collected by tornado feeder set, and discharge by star-like smooth wind device;
(3) the undesirable product after first shaping grading machine shaping classification is linked by pipeline in next shaping grading machine, carry out nodularization again and grind shaping, detect classification by proofing unit after the shaping, qualified product is collected, underproof product continues to link next shaping grading machine, i.e. circular reshaping classification successively is until qualified;
(4) by above-mentioned circular grinding shaping 6-8 hours, utilize the proofing unit classification, superfine and fines segregation in irregular shape are gone out, and collect satisfactory natural spherical plumbago;
(5) to the removal of impurities once more of satisfactory natural spherical plumbago.
2. the method for preparing natural spherical plumbago with circular reshaping classification according to claim 1, it is characterized in that: the shaping grading machine described in this method is horizontal grading machine or air-flow vortex pulverizing mill, needs 8-20 shaping grading machines in the circular reshaping classification process.
3. the method for preparing natural spherical plumbago with circular reshaping classification according to claim 1, it is characterized in that: described proofing unit comprises laser particle analyzer, microscopic imaging apparatus, density instrument and specific surface area instrument.
4. the method for preparing natural spherical plumbago with circular reshaping classification according to claim 1 is characterized in that: can adopt ultrasonic wave to the natural spherical plumbago separating impurity during removal of impurities.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863466A (en) * | 2009-11-30 | 2010-10-20 | 洛阳市冠奇工贸有限责任公司 | Automatic spheroidization device for producing spherical graphite |
| CN102951633A (en) * | 2012-11-21 | 2013-03-06 | 芜湖浙鑫新能源有限公司 | Graphite spheroidization method and production system thereby |
| US20130130117A1 (en) * | 2010-03-31 | 2013-05-23 | Sumitomo Metal Industries, Ltd. | Modified Natural Graphite Particle and Method for Producing the Same |
| CN103588194A (en) * | 2013-06-19 | 2014-02-19 | 上海捷罡机械有限公司 | Graphite ball production device based on grader and processing method of graphite ball production device |
| CN104009237A (en) * | 2014-06-09 | 2014-08-27 | 黑龙江省牡丹江农垦奥宇石墨深加工有限公司 | Ultrahigh-capacity spherical graphite cathode material and production method thereof |
| CN104425823A (en) * | 2013-09-11 | 2015-03-18 | 宁波杉杉新材料科技有限公司 | Artificial graphite cathode material of lithium ion battery and preparation method of artificial graphite cathode material |
| CN105217610A (en) * | 2015-09-10 | 2016-01-06 | 连云港江利达矿产品有限公司 | A kind of spherical graphite production technique |
| CN105776191A (en) * | 2016-02-19 | 2016-07-20 | 青岛田庄恒源石墨有限公司 | Spherical graphite production process |
| CN108176450A (en) * | 2017-12-28 | 2018-06-19 | 韦爱龄 | Graphite pulverizer |
| CN108787131A (en) * | 2018-06-01 | 2018-11-13 | 中钢集团新型材料（浙江）有限公司 | A kind of milling method of high temperature gas cooled reactor nuclear fuel element graphous graphite powder |
| CN111747405A (en) * | 2020-07-09 | 2020-10-09 | 黑龙江省宝泉岭农垦溢祥新能源材料有限公司 | Production process of spherical graphite raw material |
| CN112201377A (en) * | 2020-09-29 | 2021-01-08 | 内蒙古金彩矿业有限公司 | Shaping system and shaping method of natural graphite powder for high-temperature gas-cooled reactor nuclear fuel element |
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2008
- 2008-09-24 CN CNA2008101572816A patent/CN101367518A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863466A (en) * | 2009-11-30 | 2010-10-20 | 洛阳市冠奇工贸有限责任公司 | Automatic spheroidization device for producing spherical graphite |
| CN101863466B (en) * | 2009-11-30 | 2011-12-21 | 洛阳市冠奇工贸有限责任公司 | Automatic spheroidization device for producing spherical graphite |
| US20130130117A1 (en) * | 2010-03-31 | 2013-05-23 | Sumitomo Metal Industries, Ltd. | Modified Natural Graphite Particle and Method for Producing the Same |
| CN102951633A (en) * | 2012-11-21 | 2013-03-06 | 芜湖浙鑫新能源有限公司 | Graphite spheroidization method and production system thereby |
| CN103588194A (en) * | 2013-06-19 | 2014-02-19 | 上海捷罡机械有限公司 | Graphite ball production device based on grader and processing method of graphite ball production device |
| CN104425823B (en) * | 2013-09-11 | 2019-04-19 | 宁波杉杉新材料科技有限公司 | A kind of artificial graphite cathode material for lithium ion batteries and preparation method thereof |
| CN104425823A (en) * | 2013-09-11 | 2015-03-18 | 宁波杉杉新材料科技有限公司 | Artificial graphite cathode material of lithium ion battery and preparation method of artificial graphite cathode material |
| CN104009237A (en) * | 2014-06-09 | 2014-08-27 | 黑龙江省牡丹江农垦奥宇石墨深加工有限公司 | Ultrahigh-capacity spherical graphite cathode material and production method thereof |
| CN105217610A (en) * | 2015-09-10 | 2016-01-06 | 连云港江利达矿产品有限公司 | A kind of spherical graphite production technique |
| CN105776191A (en) * | 2016-02-19 | 2016-07-20 | 青岛田庄恒源石墨有限公司 | Spherical graphite production process |
| CN105776191B (en) * | 2016-02-19 | 2017-12-01 | 青岛田庄恒源石墨有限公司 | A kind of production technology of spherical graphite |
| CN108176450A (en) * | 2017-12-28 | 2018-06-19 | 韦爱龄 | Graphite pulverizer |
| CN108176450B (en) * | 2017-12-28 | 2019-11-05 | 吴超 | Graphite pulverizer |
| CN108787131A (en) * | 2018-06-01 | 2018-11-13 | 中钢集团新型材料（浙江）有限公司 | A kind of milling method of high temperature gas cooled reactor nuclear fuel element graphous graphite powder |
| CN108787131B (en) * | 2018-06-01 | 2020-12-08 | 中钢集团新型材料（浙江）有限公司 | Method for preparing powder from artificial graphite powder for high-temperature gas cooled reactor nuclear fuel element |
| CN111747405A (en) * | 2020-07-09 | 2020-10-09 | 黑龙江省宝泉岭农垦溢祥新能源材料有限公司 | Production process of spherical graphite raw material |
| CN112201377A (en) * | 2020-09-29 | 2021-01-08 | 内蒙古金彩矿业有限公司 | Shaping system and shaping method of natural graphite powder for high-temperature gas-cooled reactor nuclear fuel element |
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