CN101570330A - Method for preparing modified natural graphite nodules - Google Patents
Method for preparing modified natural graphite nodules Download PDFInfo
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- CN101570330A CN101570330A CNA200910019668XA CN200910019668A CN101570330A CN 101570330 A CN101570330 A CN 101570330A CN A200910019668X A CNA200910019668X A CN A200910019668XA CN 200910019668 A CN200910019668 A CN 200910019668A CN 101570330 A CN101570330 A CN 101570330A
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Abstract
The invention relates to a method for preparing modified natural graphite nodules, which is mainly used for preparing the modified natural graphite nodules. The preparation method mainly comprises the following steps: adopting a solvent, dissolving treated asphalt in the solvent in proportion to form a mixed solution, adding natural graphite nodules and the mixed solution into a reaction kettle according to certain proportion, maintaining the product at the temperature of between 60 and 70 DEG C for 3 to 4 hours, using a horizontal separator to separate solid and liquid, drying the obtained solid materials, using a crushing and classifying machine to crush the obtained solid materials, classifying materials with the particle diameter between 5 and 30 mu m, and preparing the finished products after performing curing, carbonization and graphitization treatment at a high temperature of 2,800 DEG C on the classified materials. The reversible capacity of the prepared modified natural graphite nodules reaches 350 mAh/g; the cycle index reaches 420 times; and the cycle efficiency reaches 94 percent. The products can be used for cathode materials of lithium ion secondary batteries.
Description
One, technical field:
The invention belongs to a kind of preparation method of chemical field, be mainly used in a kind of preparation of modified natural graphite nodule.
Two, background technology:
Modified natural graphite nodule belongs to new high-tech product, is mainly used in ion secondary battery cathode material lithium, and its manufacturing technology requires high.The modified natural graphite nodule poor-performing of domestic present manufacturing, the quality instability has been compared big gap with external like product, and price is higher, suddenly need a kind of high-performance, the preparation technology of modified natural graphite nodule cheaply,, meet the need of market to produce this kind product.
Three, summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of modified natural graphite nodule produces high-performance, modified natural graphite nodule cheaply, satisfies the requirement of ion secondary battery cathode material lithium.
This preparation method adopts solvent, fused with the pitch of handling by a certain percentage, form fused liquid, add natural graphite nodule and fused liquid in the reactor by a certain percentage, constant temperature 60-70 ℃, stir after 3-4 hour, to consolidate with horizontal separating machine, liquid separately, with the solids oven dry that obtains, with the crushing and classification machine break up the back material will be wherein the material classification of 5-30um go out, the good material of classification is not melted, charing, 2800 ℃ of high temperature graphitizations are handled and are made finished product, and prepared modified natural graphite nodule reversible capacity reaches 350mAh/g, cycle index 420 times, cycle efficiency 94%.
Described solvent is the mixed solution of epoxy chloropropane, purified petroleum benzin, octanol, propyl carbinol, acetone.
The proportioning of described solvent is 5: 5: 4: 4: 4.
Described pitch is dipping agent bitumen or softening temperature 75-90 ℃, quinoline insolubles＜0.5%, β-resin＞14%, the petroleum pitch of carbon residue＞50%.
Described solvent and pitch blended ratio are 50: 1.
The proportioning of described natural graphite nodule and fused liquid is 1: 5.
The main beneficial effect of present method is: owing to adopt solvent, make the fused liquid pitch of preparation be the dispersion situation, very easily form film with natural graphite nodule.
Owing to adopt dipping agent bitumen or softening temperature 75-90 ℃, quinoline insolubles＜0.5%, β-resin＞14%, the petroleum pitch of carbon residue＞50%, make macromole in the pitch, middle molecule component content lower, natural graphite nodule film after the pitch-coating is even, putamina is thinner, is convenient to interting of lithium ion.
Four, embodiment:
This preparation method is specific as follows: with solvent and pitch by 50: 1 mixed in stirring tank, constant temperature 70-80 ℃, stir after 2 hours, fused liquid of gained and the ratio of the natural graphite nodule of handling well in 5: 1 are added in the reactor, constant temperature 60-70 ℃, stir after 3-4 hour, solidliquid mixture is carried out solid-liquid separation with horizontal centrifuge, with 60 ℃ of isolated solid substance constant temperature, be incubated oven dry in 8 hours, material after the oven dry is broken up with the crushing and classification machine, classification, the material classification of 5-30um is wherein gone out, coated natural graphite ball after separating is warming up to 300 ℃ by temperature rise rate 3-4 ℃/min, after the oxidation 2 hours, must form the natural graphite nodule of oxide film, film forming natural graphite nodule is put into charring furnace, under vacuum state, be warming up to 700 ℃ by temperature rise rate 3-5 ℃/min, constant temperature carried out charing in 2 hours, and coated natural graphite ball after the charing is pressed temperature rise rate 5-10 ℃/min to 2800 ℃ under the heat insulating and sealing state, and high temperature graphitization makes reversible capacity after 2 hours and reaches 350mAh/g, cycle index 420 times, cycle efficiency 94% modified natural graphite nodule, with the modified natural graphite nodule that makes after testing after, with the vacuum-packed warehouse-in of fiber can.
Preparation method's main technique condition of a kind of modified natural graphite nodule of the present invention sees Table one
| Sequence number | Natural graphite nodule (kg) | Pitch (kg) | Epoxy chloropropane (kg) | Purified petroleum benzin (kg) | Octanol (kg) | Propyl carbinol (kg) | Acetone (kg) |
| 1 | 10 | 0.98 | 11.15 | 11.15 | 8.92 | 8.92 | 8.92 |
The technical indicator contrast table of modified natural graphite nodule of the present invention and common natural graphite nodule sees Table two
Claims (6)
1, a kind of preparation method of modified natural graphite nodule is mainly by fused liquid preparation, mix, separate, oven dry, classification, do not melt, charing, 2800 ℃ of technologies such as high temperature graphitization are formed, it is characterized in that: adopt solvent, fused with the pitch of handling by a certain percentage, form fused liquid, add natural graphite nodule and fused liquid in the reactor by a certain percentage, constant temperature 60-70 ℃, after constant temperature 3-4 hour, to consolidate with horizontal separating machine, liquid separately, with the solids oven dry that obtains, with the crushing and classification machine break up the back material will be wherein the material classification of 5-30um go out, the good material of classification is not melted, charing, 2800 ℃ of high temperature graphitizations are handled and are made finished product, prepared modified natural graphite nodule reversible capacity reaches 350mAh/g, cycle index 420 times, cycle efficiency 94%.
2, the preparation method of a kind of modified natural graphite nodule according to claim 1 is characterized in that: described solvent is the mixed solution of epoxy chloropropane, purified petroleum benzin, octanol, propyl carbinol, acetone.
3, the preparation method of a kind of modified natural graphite nodule according to claim 1 and 2 is characterized in that: the proportioning of described solvent is 5: 5: 4: 4: 4.
4, the preparation method of a kind of modified natural graphite nodule according to claim 1 is characterized in that: described pitch is dipping agent bitumen or softening temperature 75-90 ℃, quinoline insolubles＜0.5%, β-resin＞14%, the petroleum pitch of carbon residue＞50%.
5, according to the preparation method of claim 1,2,3,4 described a kind of modified natural graphite nodules, it is characterized in that: described solvent and pitch blended ratio are 50: 1.
6, the preparation method of a kind of modified natural graphite nodule according to claim 1 is characterized in that: the proportioning of described natural graphite nodule and fused liquid is 1: 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200910019668XA CN101570330A (en) | 2009-03-07 | 2009-03-07 | Method for preparing modified natural graphite nodules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200910019668XA CN101570330A (en) | 2009-03-07 | 2009-03-07 | Method for preparing modified natural graphite nodules |
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| CN101570330A true CN101570330A (en) | 2009-11-04 |
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| CNA200910019668XA Pending CN101570330A (en) | 2009-03-07 | 2009-03-07 | Method for preparing modified natural graphite nodules |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798221A (en) * | 2010-03-09 | 2010-08-11 | 武汉科技大学 | Fine texture graphite material and preparation method thereof |
| CN113410449A (en) * | 2021-06-25 | 2021-09-17 | 广东凯金新能源科技股份有限公司 | Multiphase adjustable carbon-coated novel artificial graphite negative electrode material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09251855A (en) * | 1996-03-15 | 1997-09-22 | Sumitomo Metal Ind Ltd | Manufacture of carbon powder for negative electrode of lithium ton secondary battery |
| JPH09265983A (en) * | 1996-03-29 | 1997-10-07 | Petoca:Kk | Manufacture of graphite milled fibers to be used as negative electrode material for lithium ion secondary battery |
| CN1792783A (en) * | 2005-11-29 | 2006-06-28 | 冷亮 | Process for preparing modified natural graphite nodule |
| CN101108729A (en) * | 2006-07-20 | 2008-01-23 | 天津市铁诚电池材料有限公司 | Method for manufacturing artificial plumbago negative pole material of lithium ion power cell |
-
2009
- 2009-03-07 CN CNA200910019668XA patent/CN101570330A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09251855A (en) * | 1996-03-15 | 1997-09-22 | Sumitomo Metal Ind Ltd | Manufacture of carbon powder for negative electrode of lithium ton secondary battery |
| JPH09265983A (en) * | 1996-03-29 | 1997-10-07 | Petoca:Kk | Manufacture of graphite milled fibers to be used as negative electrode material for lithium ion secondary battery |
| CN1792783A (en) * | 2005-11-29 | 2006-06-28 | 冷亮 | Process for preparing modified natural graphite nodule |
| CN101108729A (en) * | 2006-07-20 | 2008-01-23 | 天津市铁诚电池材料有限公司 | Method for manufacturing artificial plumbago negative pole material of lithium ion power cell |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798221A (en) * | 2010-03-09 | 2010-08-11 | 武汉科技大学 | Fine texture graphite material and preparation method thereof |
| CN101798221B (en) * | 2010-03-09 | 2012-10-10 | 武汉科技大学 | Fine texture graphite material and preparation method thereof |
| CN113410449A (en) * | 2021-06-25 | 2021-09-17 | 广东凯金新能源科技股份有限公司 | Multiphase adjustable carbon-coated novel artificial graphite negative electrode material and preparation method thereof |
| CN113410449B (en) * | 2021-06-25 | 2022-08-02 | 广东凯金新能源科技股份有限公司 | Multiphase adjustable carbon-coated artificial graphite negative electrode material and preparation method thereof |
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Application publication date: 20091104 |