CN106410196A - Improved low-temperature surface modification process and application of synthetic graphite material - Google Patents
Improved low-temperature surface modification process and application of synthetic graphite material Download PDFInfo
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- CN106410196A CN106410196A CN201510535391.1A CN201510535391A CN106410196A CN 106410196 A CN106410196 A CN 106410196A CN 201510535391 A CN201510535391 A CN 201510535391A CN 106410196 A CN106410196 A CN 106410196A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Engineering & Computer Science (AREA)
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- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
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Abstract
The invention discloses an improved low-temperature surface modification process and application of a synthetic graphite material. The process comprises the following steps: firstly, shortening the width of an inner helical ribbon of an original reaction still stirrer by 20 to 40 mm, and increasing the quantity of scarping knives on an outer helical ribbon by 6 to 10; putting the synthetic graphite material into a modified reaction still for carrying out warming modification, wherein the modified constant-temperature temperature is 600 to 650 DEG C, the constant-temperature time is 280 to 320 min, and the modified treatment total time is 500 to 560 min; secondly, according to conditions in the first step, adjusting the stirring rotating speed of the reaction still to be 12 to 14 r/min for carrying out modification; thirdly, according to the conditions in the first step, adjusting the stirring rotating speed of the reaction still to be 21 to 23 r/min for carrying out modification; and fourthly, according to the conditions in the first step, adjusting the stirring rotating speed of the reaction still to be 38 to 40 r/min for carrying out modification. The volatile matter of the synthetic graphite material is reduced, the tap density is improved, and the processability of the material is not influenced.
Description
Technical field
The present invention relates to material modification processing technology field, the low temperature of specifically a kind of improved artificial graphite material
Surface modification technology and application.
Background technology
In recent years, the progress of the development with the epoch and science and technology, electronic product universalness, consumer is to electricity
The service life in pond, energy density and safety more are paid close attention to.Therefore, some serviceabilities are good and energy
The high battery material of density is extensively studied.Particularly the research to lithium ion battery in recent years is it is desirable to have
Higher energy density, more preferable serviceability.At present, in field of lithium, have been directed towards improving battery
Serviceability, the battery obtaining higher-capability density conducts extensive research, continuous however as electronic product
Update, the performance requirement of battery also improved further, this is accomplished by improving the tap density of battery material,
Thus improving the performance of Delanium battery.
At present in Delanium produces, the product for some surface modification treatment has been widely developed
And application, but there is a weak point, in processing, the tap density of material is low, as everybody knows artificial stone
During ink material following process, graphitization can be carried out, these low tap density materials carry out shaking after graphitization
Real density also can be relatively low, so the serviceability that improve lithium battery can must be had an impact.
In the processing of artificial graphite material, typically carry out surface modification treatment to improve the tap density of material.
Tap density refers to the quality of powder measured unit volume after jolt ramming in container under certain condition.So
The tap density of material should be improved as far as possible in modification, thus ensureing that lithium battery product has higher serviceability.
Content of the invention
It is an object of the invention to provide a kind of low-temperature surface modified technique of improved artificial graphite material and should
With, the technological parameter in being processed by adjustment, make improvements and optimize, in the processability not affecting product
It is ensured that artificial graphite material obtains relatively more in modification under the premise of energy, the safety and stability of material
High, more stable tap density.
For achieving the above object, the present invention provides following technical scheme：
A kind of low-temperature surface modified technique of improved artificial graphite material, comprises the following steps：
1. first reactor agitator is transformed：The interior ribbon width of original reactor agitator is shortened
20～40mm, the scraper quantity on outer ribbon is increased by 6～10；Then artificial graphite material is put into and change
Carry out the modification that heats up, at 600 DEG C～650 DEG C, constant temperature time exists modified thermostat temperature in reactor after making
280～320min, modification total time is 500～560min；
2. the condition 1. according to step, reactor speed of agitator is adjusted to 12～14r/min and is modified, raw
Produce quantity 3 kettle；
3. the condition 1. according to step, reactor speed of agitator is adjusted to 21～23r/min and is modified, raw
Produce quantity 3 kettle；
4. the condition 1. according to step, reactor speed of agitator is adjusted to 38～40r/min and is modified, raw
Produce quantity 3 kettle.
As the further scheme of the present invention：Described step 1. in, the width of interior ribbon shortens 40mm, outer spiral shell
Scraper quantity on band increases by 8, and described artificial graphite material is various common artificial stone conventional in the art
Ink material, the modified dosage of each low-temperature surface of artificial graphite material is 650～700kg.
As the further scheme of the present invention：Described step 1. in, each low-temperature surface of artificial graphite material is modified
The dosage processing is 675kg.
As the further scheme of the present invention：Described step 1. in, the modified particle diameter of artificial graphite material is
D50 volume average particle size is at 15～23 μm.
As the further scheme of the present invention：Described step 1. in, the modified particle diameter of artificial graphite material is
D50 volume average particle size is at 16～19 μm.
As the further scheme of the present invention：Described step 1. in, described artificial graphite material low-temperature surface changes
Property process thermostat temperature at 650 DEG C, constant temperature time is preferably 300min, and constant temperature time is most preferably 320min,
Modification total time is 500～560min.
As the further scheme of the present invention：Described step 2. in, described reactor speed of agitator be 13r/min.
As the further scheme of the present invention：Described step 3. in, described reactor speed of agitator be 22r/min.
As the further scheme of the present invention：Described step 4. in, described reactor speed of agitator be 39r/min.
The low-temperature surface modified technique of described improved artificial graphite material answering in lithium cell cathode material
With.
The present invention is to provide application in modification for the artificial graphite material.
The present invention is to provide a kind of artificial graphite material the changing of technological parameter in preparing lithium cell cathode material
Enter, be that product is more stable, optimize product.Described lithium battery material refers generally to lithium cell cathode material.
Reagent used by the present invention and raw material are all commercially available.
Compared with prior art, the invention has the beneficial effects as follows：1. after increase scraper reduction material is heated, anti-
Answer the problem of buildup on the kettle wall of kettle；2. ribbon width in shortening, prevents solid accumulation, increases material movement certainly
By property, make material coat evenly, finer and close；3. the volatile matters of modified material are reduced；4. tap density is bright
Aobvious raising；5. overall particle size distribution will not be impacted, and size particles are more evenly distributed；6. modified product
Matter is stable, optimizes the performance indications of product.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clearly and completely
Description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.
Based on the embodiment in the present invention, those of ordinary skill in the art are obtained under the premise of not making creative work
The every other embodiment obtaining, broadly falls into the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of low-temperature surface modified technique of improved artificial graphite material, including following
Step：
1. artificial graphite material 675kg is put into and in reactor, carry out the modification that heats up, modified thermostat temperature exists
600 DEG C, in 280min, modification total time is 500min to constant temperature time；
2. the condition 1. according to step, reactor speed of agitator is adjusted to 12r/min and is modified, and produces number
Measure 3 kettles；
3. the condition 1. according to step, reactor speed of agitator is adjusted to 21r/min and is modified, and produces number
Measure 3 kettles；
4. the condition 1. according to step, reactor speed of agitator is adjusted to 38r/min and is modified, and produces number
Measure 3 kettles.
The material result produced according to this technique is as follows：
Step 2. technological parameter final load 612.02kg, yield 90.67%, particle diameter D10：7.07 μm,
Particle diameter D50：18.93 μm, particle diameter D90：46.84 μm, particle diameter D99：171.67 μm, particle diameter Dmax：
309.07 μm, tap density 0.65g/cm3, volatile matters 7.66%.
Step 3. technological parameter final load 606.55kg, yield 89.86%, particle diameter D10：8.93 μm,
Particle diameter D50：19.04 μm, particle diameter D90：39.52 μm, particle diameter D99：121.58 μm, particle diameter Dmax：
195.41 μm, tap density 0.71g/cm3, volatile matters 6.11%.
Step 4. technological parameter final load 602.37kg, yield 89.24%, particle diameter D10：8.93 μm,
Particle diameter D50：19.77 μm, particle diameter D90：58.07 μm, particle diameter D99：168.27 μm, particle diameter Dmax：
274.63 μm, tap density 0.76g/cm3, volatile matters 5.30%.
Embodiment 2
In the embodiment of the present invention, a kind of low-temperature surface modified technique of improved artificial graphite material, including following
Step：
1. artificial graphite material 675kg is put into and in reactor, carry out the modification that heats up, modified thermostat temperature exists
625 DEG C, in 300min, modification total time is 560min to constant temperature time；
2. the condition 1. according to step, reactor speed of agitator is adjusted to 14r/min and is modified, and produces number
Measure 3 kettles；
3. the condition 1. according to step, reactor speed of agitator is adjusted to 23r/min and is modified, and produces number
Measure 3 kettles；
4. the condition 1. according to step, reactor speed of agitator is adjusted to 40r/min and is modified, and produces number
Measure 3 kettles.
The material result produced according to this technique is as follows：
Step 2. technological parameter final load 609.80kg, yield 90.34%, particle diameter D10：7.11 μm,
Particle diameter D50：18.87 μm, particle diameter D90：48.64 μm, particle diameter D99：183.24 μm, particle diameter Dmax：
298.98 μm, tap density 0.66g/cm3, volatile matters 7.04%.
Step 3. technological parameter final load 605.95kg, yield 89.77%, particle diameter D10：8.87 μm,
Particle diameter D50：19.18 μm, particle diameter D90：40.78 μm, particle diameter D99：208.64 μm, particle diameter Dmax：
306.31 μm, tap density 0.72g/cm3, volatile matters 5.75%.
Step 4. technological parameter final load 602.64kg, yield 89.28%, particle diameter D10：9.01 μm,
Particle diameter D50：19.65 μm, particle diameter D90：50.37 μm, particle diameter D99：225.38 μm, particle diameter Dmax：
315.37 μm, tap density 0.75g/cm3, volatile matters 5.03%.
Embodiment 3
In the embodiment of the present invention, a kind of low-temperature surface modified technique of improved artificial graphite material, including following
Step：
1. artificial graphite material 675kg is put into and in reactor, carry out the modification that heats up, modified thermostat temperature exists
650 DEG C, in 320min, modification total time is 550min to constant temperature time；
2. the condition 1. according to step, reactor speed of agitator is adjusted to 13r/min and is modified, and produces number
Measure 3 kettles；
3. the condition 1. according to step, reactor speed of agitator is adjusted to 22r/min and is modified, and produces number
Measure 3 kettles；
4. the condition 1. according to step, reactor speed of agitator is adjusted to 39r/min and is modified, and produces number
Measure 3 kettles.
The material result produced according to this technique is as follows：The step 2. final load of technological parameter
610.06kg, yield 90.38%, particle diameter D10：7.54 μm, particle diameter D50：18.58 μm, particle diameter D90：
49.37 μm, particle diameter D99：197.23 μm, particle diameter Dmax：305.24 μm, tap density 0.65g/cm3,
Volatile matters 6.78%.Step 3. technological parameter final load 603.25kg, yield 89.37%, particle diameter D10：
8.91 μm, particle diameter D50：19.68 μm, particle diameter D90：48.78 μm, particle diameter D99：208.77 μm,
Particle diameter Dmax：297.68 μm, tap density 0.71g/cm3, volatile matters 5.34%.Step 4. technological parameter
Final load 607.29kg, yield 89.97%, particle diameter D10：9.01 μm, particle diameter D50：19.87 μm,
Particle diameter D90：51.37 μm, particle diameter D99：232.54 μm, particle diameter Dmax：328.79 μm, tap density
0.75g/cm3, volatile matters 4.67%.
The present invention has advantages below：1. after increase scraper reduction material is heated, buildup on the kettle wall of reactor
Problem；2. ribbon width in shortening, prevents solid accumulation, increases material movement freedom, so that material is coated
Evenly, finer and close；3. the volatile matters of modified material are reduced；4. tap density significantly improves；5. overall grain
Degree distribution will not be impacted, and size particles are more evenly distributed；6. modified product property is stable, optimizes product
Performance indications.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and
And without departing from the spirit or essential characteristics of the present invention, can be realized this in other specific forms
Bright.Therefore, no matter from the point of view of which point, embodiment all should be regarded as exemplary, and be non-limiting
, the scope of the present invention is limited by claims rather than described above, it is intended that will fall will in right
All changes in the implication and scope of the equivalency asked are included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment party
Formula only comprises an independent technical scheme, this narrating mode of description only for clarity, ability
Field technique personnel should be using description as an entirety, and the technical scheme in each embodiment can also be through suitable group
Close, formed it will be appreciated by those skilled in the art that other embodiment.
Claims (10)
1. a kind of low-temperature surface modified technique of improved artificial graphite material is it is characterised in that include following walking
Suddenly：
1. first reactor agitator is transformed：The interior ribbon width of original reactor agitator is shortened
20～40mm, the scraper quantity on outer ribbon is increased by 6～10；Then artificial graphite material is put into and change
Carry out the modification that heats up, at 600 DEG C～650 DEG C, constant temperature time exists modified thermostat temperature in reactor after making
280～320min, modification total time is 500～560min；
2. the condition 1. according to step, reactor speed of agitator is adjusted to 12～14r/min and is modified；
3. the condition 1. according to step, reactor speed of agitator is adjusted to 21～23r/min and is modified；
4. the condition 1. according to step, reactor speed of agitator is adjusted to 38～40r/min and is modified.
2. the low-temperature surface modified technique of improved artificial graphite material according to claim 1, its feature
Be, described step 1. in, the width of interior ribbon shortens 40mm, and the scraper quantity on outer ribbon increases by 8,
The modified dosage of each low-temperature surface of artificial graphite material is 650～700kg.
3. the low-temperature surface modified technique of improved artificial graphite material according to claim 1, its feature
Be, described step 1. in, the dosage of artificial graphite material each low-temperature surface modification is 675kg.
4. the low-temperature surface modified technique of improved artificial graphite material according to claim 3, its feature
Be, described step 1. in, the modified particle diameter of artificial graphite material be D50 volume average particle size 15～
23μm.
5. the low-temperature surface modified technique of improved artificial graphite material according to claim 1, its feature
Be, described step 1. in, the modified particle diameter of artificial graphite material be D50 volume average particle size 16～
19μm.
6. the low-temperature surface modified technique of improved artificial graphite material according to claim 1, its feature
Be, described step 1. in, the thermostat temperature of described artificial graphite material low-temperature surface modification exists
650 DEG C, in 320min, modification total time is 500～560min to constant temperature time.
7. the low-temperature surface modified technique of improved artificial graphite material according to claim 1, its feature
Be, described step 2. in, described reactor speed of agitator be 13r/min.
8. the low-temperature surface modified technique of improved artificial graphite material according to claim 1, its feature
Be, described step 3. in, described reactor speed of agitator be 22r/min.
9. the low-temperature surface modified technique of improved artificial graphite material according to claim 1, its feature
Be, described step 4. in, described reactor speed of agitator be 39r/min.
10. low-temperature surface modified technique according to the arbitrary described improved artificial graphite material of claim 1～9
Application is it is characterised in that apply in lithium cell cathode material.
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| CN201510535391.1A CN106410196A (en) | 2015-08-27 | 2015-08-27 | Improved low-temperature surface modification process and application of synthetic graphite material |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009013761A1 (en) * | 2007-07-23 | 2009-01-29 | Satbir Singh | Smart double ribbon screw mixer |
| CN102921366A (en) * | 2011-08-11 | 2013-02-13 | 许洪军 | Helical ribbon type reaction kettle with double stirrers arranged at top and bottom |
| 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 |
| CN204234004U (en) * | 2014-11-06 | 2015-04-01 | 中联重科物料输送设备有限公司 | Mixer |
| CN104600309A (en) * | 2014-12-29 | 2015-05-06 | 东莞市凯金新能源科技有限公司 | Preparation method of secondary start-up lithium ion battery cathode material |
-
2015
- 2015-08-27 CN CN201510535391.1A patent/CN106410196A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009013761A1 (en) * | 2007-07-23 | 2009-01-29 | Satbir Singh | Smart double ribbon screw mixer |
| CN102921366A (en) * | 2011-08-11 | 2013-02-13 | 许洪军 | Helical ribbon type reaction kettle with double stirrers arranged at top and bottom |
| 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 |
| CN204234004U (en) * | 2014-11-06 | 2015-04-01 | 中联重科物料输送设备有限公司 | Mixer |
| CN104600309A (en) * | 2014-12-29 | 2015-05-06 | 东莞市凯金新能源科技有限公司 | Preparation method of secondary start-up lithium ion battery cathode material |
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