CN102354745A - Manufacturing method of lithium-ion battery cathode material and lithium-ion battery cathode material prepared by manufacturing method - Google Patents
Manufacturing method of lithium-ion battery cathode material and lithium-ion battery cathode material prepared by manufacturing method Download PDFInfo
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- CN102354745A CN102354745A CN2011102451350A CN201110245135A CN102354745A CN 102354745 A CN102354745 A CN 102354745A CN 2011102451350 A CN2011102451350 A CN 2011102451350A CN 201110245135 A CN201110245135 A CN 201110245135A CN 102354745 A CN102354745 A CN 102354745A
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Abstract
The invention belongs to the field of energy and discloses a manufacturing method of a lithium-ion battery cathode material and the lithium-ion battery cathode material prepared by the manufacturing method. The manufacturing method comprises the following steps of: (1) uniformly mixing a mixture and an adhesive material with the weight ratio of the micropowder to the adhesive material being 1:0.01-0.5, wherein the mixture contains one or more micropowders selected from a graphite micropowder, a coke micropowder or a burning coke micropowder with the mean particle size being 1-7 microns; (2) carrying out heat treatment on the mixture in step (1) isolated from air at the temperature of 500-1500 DEG C to obtain a solid material; (3) crushing and grading the obtained solid material to obtain carbonaceous intermediate particles which satisfy the requirement of the lithium-ion battery cathode material on the particle size; (4) carrying out graphitization on the carbonaceous intermediate particles obtained from the step (3) at the temperature of 2200-3200 DEG C. The manufacturing method of the lithium-ion battery cathode material has advantages of low production cost, simple technology and good processing performance. The battery made from the lithium-ion battery cathode material has cyclic stability and excellent rate performance. In addition, the utility value of the graphite micropowder, the coke micropowder or the burning coke micropowder is raised.
Description
Technical field
The present invention relates to lithium ion battery negative material.
Background technology
With petroleum coke (containing green coke, ripe Jiao) and graphite product is that existing many pieces of related patent U.S. Patent No. of manufacturing approach of feedstock production lithium ion battery negative material are delivered, and belongs to known technology, and wherein much commercialization has been for many years.Numerous lithium ion battery negative material manufacturer, having adopted with the above-mentioned material is that the production technology of raw material is carried out the production of lithium ion battery negative material on a large scale.Wherein most preparation technologies all need pulverize earlier above-mentioned raw materials, then go out the carbonaceous intermediate that on particle size distribution, meets as negative pole through fractionated.And in crushing process, exist a part of raw material inevitably and cross to be pulverized (proportion 30～70% does not wait), these crossed the raw material pulverized since particle diameter too small-average grain diameter 1～7 μ m, that vibration density is spent is low-at 0.5g/cm
3Below; Suitable directly as intermediate products entering next procedure production lithium ion battery negative material; Therefore to separate through means such as classifications; The raw material that these that separate are crossed pulverizing has withdrawed from the production process of negative material, thereby has produced a large amount of micro mist byproducts, and its actual scale scale with major product approximately is suitable.The difference of corresponding raw material, these micro mist byproducts are called green coke micro mist, ripe burnt micro mist and graphite microparticles respectively, and they can only be sold carbon element enterprise as useless carbon dust and make the lower low side carbon product of some added values at present, so selling price is very cheap.Because these useless carbon dust bulk densities are very low, its packing, freight are also very high, thereby have further compressed profit margin.
Lithium ion battery market development in recent years is rapid.Form communication apparatus power supply, electrical source of power, three bursts of powerful motive forces of redundant electrical power, its economic scale every year is with 16% speed increment.Closely bound up with it negative material industry is in the rising passway of a long-term high speed development at present.The power-type lithium ion battery that is used for electric bicycle, electric automobile is that country supports development rapidly under the policy guidance of new-energy automobile energetically.Because the particularity of its application industry of Vehicular dynamic battery, the negative material that adapts with it must reach higher level on economy, multiplying power property and cyclical stability.Therefore exploitation is more low-cost, more the negative material of the forthright and better stable circulation type of high power is an important topic of present negative pole exploitation.
Summary of the invention
The object of the present invention is to provide a kind of byproduct to produce in the lithium ion battery negative material production process---graphite microparticles or green coke micro mist or ripe burnt micro mist are primary raw material, prepare the method for lithium ion battery negative material.
The present invention adopts following technical scheme: a kind of manufacturing approach of lithium ion battery negative material comprises following process:
(1) with one or more the mixture of average grain diameter in the graphite microparticles of 1～7 μ m, green coke micro mist or ripe burnt micro mist, with binding material by micro mist: binding material is that 1: 0.01～0.5 weight ratio mixes;
(2) the mixture secluding air in (1) is heat-treated under 500～1500 ℃, obtain the solid bodies type material;
(3) the solid bodies type material that obtains is pulverized and classification, obtained the carbonaceous mesophase body that average grain diameter meets the lithium ion battery negative material requirement;
(4) (3) gained carbonaceous mesophase body is carried out graphitization processing under 2200～3200 ℃, be lithium ion battery negative material.
Can also adopt following method, particularly be raw material with the graphite microparticles, to simplify technology and to reduce cost:
(1) with average grain diameter at the graphite microparticles of 1～7 μ m and binding material by micro mist: binding material is that 1: 0.01～0.5 weight ratio mixes;
(2) (1) gained mixture is carried out the charing processing under 800～2200 ℃ of conditions and obtain solid carbonaceous bulk material;
(3) with the solid carbonaceous bulk material of (2) gained pulverize, classification, obtain the carbonaceous powder that average grain diameter meets the lithium ion battery negative material requirement.
The mixing of the preferred coal tar pitch of said bonding agent, petroleum asphalt, coal tar or above composition; These materials itself have viscosity can do the bonding agent use; Simultaneously be easy to charing and graphitization processing again, can form the graphite-like charcoal after the processing, this part charcoal can be made contributions to the capacity of battery.And the resinae organic binder bond can't form graphite matter carbon, though little to the battery capacity contribution, good stability helps providing cycle-index.
The present invention also provides the lithium ion battery negative material that obtains with said method production.
Method of the present invention prepares lithium ion battery negative material; Have following beneficial effect: with the accessory substance micro mist that produces in the lithium ion battery production process is raw material; Production cost is low, technology is simple, processing characteristics is good, and with its battery stable circulation of making, high rate performance is outstanding; And improved the value of graphite microparticles, green coke micro mist or ripe burnt micro mist, improved resource utilization.
Embodiment
Through specific embodiment the present invention is described in further detail below.
One, the embodiment of graphitization processing
With the green coke micro mist of average grain diameter 4～5 μ m, ripe burnt micro mist or graphite differential, mixing in proportion with petroleum asphalt, coal tar pitch or coal tar, after mixing, heat treatment certain hour under the mixture secluding air condition obtains the solid bodies type material; The solid bodies type material that obtains is pulverized and classification, obtained the carbonaceous mesophase body that average grain diameter meets the requirement of lithium ion battery negative material particle diameter; Gained carbonaceous mesophase body is carried out graphitization processing, be lithium ion battery negative material.Concrete process conditions are seen embodiment 1-5 in the table 1.
Two, the embodiment of charing processing
With the graphite microparticles of average grain diameter 4～5 μ m, with petroleum asphalt by micro mist: petroleum asphalt is that 1: 0.18 weight ratio mixes under 250 ℃ of conditions; Mixture is carried out the charing processing obtain solid carbonaceous bulk material under 1200 ℃ of conditions; The solid carbonaceous bulk material of gained is pulverized, classification, obtains the 14.75 μ m carbonaceous powders that average grain diameter meets particle diameter that lithium cell cathode material requires, and is lithium ion battery negative material, and concrete process conditions are seen embodiment 6 in the table 1.
The concrete technology of the different embodiment of table 1
Experimental example
Be the performance of testing product,, properties of product detected according to the conventional evaluating testing method of lithium ion battery negative material with product among the embodiment 1-6 and comparative sample 1-3.
Used comparative sample is:
Comparative sample 1: green coke micro mist
Comparative sample 2: ripe burnt micro mist
Comparative sample 3: stone is deceived micro mist
The result sees table 2
. table 2 different materials properties of product
Experimental result by embodiment and Comparative Examples is visible; The accessory substance that tradition negative pole material manufacture enterprise system produces when producing: green coke micro mist, ripe burnt micro mist and graphite microparticles, can average grain diameter be brought up to 10.45～14.75 μ m by 4.23～4.86 μ m via this method; With tap density by 0.43～0.45gcm
-3Bring up to 0.95～1.12gcm
-3, with specific area by 17.07～19.34m
2g
-1Drop to 1.7～2.4m
2g
-1Processing characteristics can't be made battery to be improved to processing characteristics good by original, and has higher gram volume (332～350mAhg
-1) and with good high rate performance (10 multiplying powers are 79.6～85.4%; 20 multiplying powers are 69.4～73.3%) and cyclical stability (80% capacity cycle life is at 740～956 times).
Claims (7)
1. the manufacturing approach of a lithium ion battery negative material comprises following process:
(1) with one or more the mixture of average grain diameter in the graphite microparticles of 1～7 μ m, green coke micro mist or ripe burnt micro mist, with binding material by micro mist: binding material is that 1: 0.01～0.5 weight ratio mixes;
(2) the mixture secluding air in (1) is heat-treated under 500～1500 ℃, obtain the solid bodies type material;
(3) the solid bodies type material that obtains is pulverized and classification, obtained meeting the carbonaceous mesophase body particle of lithium ion battery negative material particle diameter requirement;
(4) (3) gained carbonaceous mesophase body particle is carried out graphitization processing under 2200～3200 ℃.
2. the method for claim 1, it is characterized in that: said binding agent is coal tar pitch, oil drop. the mixing of blue or green, coal tar or above composition.
3. according to claim 1 or claim 2 method, it is characterized in that: the average grain diameter of said carbonaceous mesophase body particle is 5～45 μ m behind the crushing and classification.
4. the manufacturing approach of a lithium ion battery negative material comprises following process:
(1) with average grain diameter at the graphite microparticles of 1～7 μ m and binding material by micro mist: binding material is that 1: 0.01～0.5 weight ratio mixes;
(2) (1) gained mixture is carried out the charing processing under 800～2200 ℃ of conditions and obtain solid carbonaceous bulk material;
(3) with the solid carbonaceous bulk material of (2) gained pulverize, classification, obtain the carbonaceous powder that average grain diameter meets the lithium ion battery negative material requirement.
5. method as claimed in claim 4 is characterized in that: said binding agent is the mixing of coal tar pitch, petroleum asphalt, coal tar or above composition.
6. like claim 4 or 5 described methods, it is characterized in that: the average grain diameter of said carbonaceous mesophase body particle is 5～45 μ m.
7. the lithium ion battery negative material of claim 1 or 4 said methods preparations.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482606A (en) * | 2013-09-23 | 2014-01-01 | 辽宁弘光科技(集团)有限公司 | Production method for intermediate phase carbon anode material |
| CN103682350A (en) * | 2013-12-25 | 2014-03-26 | 东莞市凯金新能源科技有限公司 | Preparation method of asphalt liquid phase coated modified artificial graphite lithium battery cathode material |
| CN103840161A (en) * | 2013-12-19 | 2014-06-04 | 东莞市凯金新能源科技有限公司 | Method for preparing lithium battery negative electrode material, and lithium battery negative electrode sheet |
| CN104362299A (en) * | 2014-10-24 | 2015-02-18 | 中国海洋石油总公司 | Preparation method of artificial graphite anode material |
| CN104766955A (en) * | 2015-04-24 | 2015-07-08 | 田东 | Method for recycling natural graphite fine powder as negative pole material |
| CN106935857A (en) * | 2017-03-17 | 2017-07-07 | 雅安乾润锂电池材料有限公司 | A kind of ultrafine graphite cathode material |
| CN110071274A (en) * | 2019-04-19 | 2019-07-30 | 平顶山东方碳素股份有限公司 | Coat the processing technology that facture improves artificial plumbago negative pole material performance |
| CN110718690A (en) * | 2018-07-12 | 2020-01-21 | 宝武炭材料科技有限公司 | Preparation method of battery negative electrode material based on needle coke green coke and calcined coke |
| CN112768690A (en) * | 2021-01-15 | 2021-05-07 | 内蒙古恒科新材料科技有限公司 | Preparation method for recycling lithium ion battery negative electrode material from waste graphite crucible |
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| CN1885598A (en) * | 2006-07-10 | 2006-12-27 | 深圳市贝特瑞电子材料有限公司 | Composite carbon negative electrode material of lithium ion power battery and its preparation method |
| US20100021370A1 (en) * | 2008-07-25 | 2010-01-28 | Devarayasamudram Ramachandran Nagaraj | Flotation Reagents and Flotation Processes Utilizing Same |
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| CN1885598A (en) * | 2006-07-10 | 2006-12-27 | 深圳市贝特瑞电子材料有限公司 | Composite carbon negative electrode material of lithium ion power battery and its preparation method |
| US20100021370A1 (en) * | 2008-07-25 | 2010-01-28 | Devarayasamudram Ramachandran Nagaraj | Flotation Reagents and Flotation Processes Utilizing Same |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103482606B (en) * | 2013-09-23 | 2015-06-17 | 大连宏光锂业股份有限公司 | Production method for intermediate phase carbon anode material |
| CN103482606A (en) * | 2013-09-23 | 2014-01-01 | 辽宁弘光科技(集团)有限公司 | Production method for intermediate phase carbon anode material |
| CN103840161B (en) * | 2013-12-19 | 2017-01-04 | 东莞市凯金新能源科技股份有限公司 | A kind of method preparing lithium cell cathode material and lithium battery cathode plate |
| CN103840161A (en) * | 2013-12-19 | 2014-06-04 | 东莞市凯金新能源科技有限公司 | Method for preparing lithium battery negative electrode material, and lithium battery negative electrode sheet |
| CN103682350A (en) * | 2013-12-25 | 2014-03-26 | 东莞市凯金新能源科技有限公司 | Preparation method of asphalt liquid phase coated modified artificial graphite lithium battery cathode material |
| CN103682350B (en) * | 2013-12-25 | 2014-07-23 | 东莞市凯金新能源科技有限公司 | Preparation method of asphalt liquid phase coated modified artificial graphite lithium battery cathode material |
| CN104362299A (en) * | 2014-10-24 | 2015-02-18 | 中国海洋石油总公司 | Preparation method of artificial graphite anode material |
| CN104766955A (en) * | 2015-04-24 | 2015-07-08 | 田东 | Method for recycling natural graphite fine powder as negative pole material |
| CN106935857A (en) * | 2017-03-17 | 2017-07-07 | 雅安乾润锂电池材料有限公司 | A kind of ultrafine graphite cathode material |
| CN110718690A (en) * | 2018-07-12 | 2020-01-21 | 宝武炭材料科技有限公司 | Preparation method of battery negative electrode material based on needle coke green coke and calcined coke |
| CN110718690B (en) * | 2018-07-12 | 2022-07-12 | 宝武碳业科技股份有限公司 | Preparation method of battery negative electrode material based on needle coke green coke and calcined coke |
| CN110071274A (en) * | 2019-04-19 | 2019-07-30 | 平顶山东方碳素股份有限公司 | Coat the processing technology that facture improves artificial plumbago negative pole material performance |
| CN112768690A (en) * | 2021-01-15 | 2021-05-07 | 内蒙古恒科新材料科技有限公司 | Preparation method for recycling lithium ion battery negative electrode material from waste graphite crucible |
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Application publication date: 20120215 |