CN109860524A - A kind of method of solid asphalt low temperature cladding preparation negative electrode material - Google Patents
A kind of method of solid asphalt low temperature cladding preparation negative electrode material Download PDFInfo
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Abstract
The invention discloses a kind of methods that solid asphalt low temperature coats preparation negative electrode material, comprising: with one of needle coke, pitch coke coke powder for raw material；It crushes: being crushed needle coke with airslide disintegrating mill, D50 is at 8~18 μm；Graphitization: 2800~3000 DEG C of graphitization temperature；Cladding: graphous graphite powder and high softening point bitumen powder are added in coating reaction kettle and mix cladding；High softening point bitumen additional amount 3%~15wt%, needle-shaped 85%~97wt% of coke powder；Temperature of plate: 270~300 DEG C, 1~2h of time is coated；The mixture coated is carbonized into 1-3h under 700-1000 DEG C of temperature, nitrogen atmosphere, is sieved after being cooled to room temperature, prepares high performance lithium ion battery negative material.Negative electrode material prepared by the present invention takes off lithium capacity for the first time, and coulombic efficiency is more than 350mAh/g for the first time, and coulombic efficiency is up to 92% or more for the first time, superior performance.Therefore, the negative electrode material simple process prepared with this method, production cost is low and has high-performance.
Description
Technical field
The present invention relates to cell negative electrode material manufacturing fields, and in particular to a kind of side that negative electrode material is prepared using coke powder
Method.
Background technique
As power battery is to the capacity of negative electrode material, cyclicity and forthright requirement continuous improvement again, natural graphite is compared
Negative electrode material, artificial plumbago negative pole material have more excellent performance, and artificial plumbago negative pole material has become power battery cathode
The mainstream of material.Currently, being used to prepare the raw material of artificial graphite Li-like ions cell negative electrode material mainly has: needle coke, petroleum
Burnt, pitch coke.Because graphite is poor with solvent compatibility, high rate during charging-discharging is bad, because of solvent molecule when first charge-discharge
Insertion keeps graphite linings easily peeling-off altogether, so as to cause battery cycle life reduction.Therefore it needs to carry out graphite material surface
Modification, the specific surface area by suitably reducing graphite reduce because the irreversible capacity caused by forming excessive SEI film damages
Lose and solvent molecule total insertion and cause graphite linings to be removed；And by modifying graphite surface, make its superficiality
Matter is uniform, avoids Topically active is excessively high solvent is caused acutely to decompose caused irreversible loss.Surface treatment method mainly has
Coating modification, doping vario-property, gas phase fluorination, plasma treatment, sour processing, mechanical lapping, reduction etc..
Currently, common surface modifying method is mainly coating modification in industrialized production.It is " a kind of to prepare in patent document
In the method and lithium battery cathode plate of lithium cell cathode material ", first by after crushing and classification needle coke powder and pitch powder into
Row mixing, uniformly mixed powder, which is put into, reacts 5~10h in 500~650 DEG C of medium temperature reaction kettle, is then graphitized
Processing.It is coated again with the pitch tetrahydrofuran solution prepared after graphitization processing, the lithium electricity of pitch-coating is made through carbonizing
Pond negative electrode material.The method reaction temperature is high, and the reaction time is also longer, and process flow is long and complicated, is unfavorable for low-cost industrial
Produce lithium cell cathode material.And in patent document " ion secondary battery cathode material lithium and preparation method thereof ", using day
The mixture of right graphite and Raw needle coke powder is raw material, and asphalt powder is added and carries out hot place at 300~700 DEG C after mixing
Reason finally carries out graphitization processing at 2500~2800 DEG C and lithium cell cathode material is made.This method is with natural graphite and needle
Shape coke coking powder be raw material, comparatively, by artificial graphite be raw material preparation power battery negative electrode material comprehensive performance more
Good, the method heat treatment temperature is also higher, increases production cost.And it first carbonizes and is graphitized afterwards, be unfavorable for generating " core-shell structure copolymer " structure
Performance preferably negative electrode material.
Summary of the invention
Therefore, the technical problem to be solved by the present invention is to providing one kind can be generated " core-shell structure copolymer " structure, and simple process is raw
Produce negative electrode material at low cost and with high performance.
The technical scheme is that a kind of method of solid asphalt low temperature cladding preparation negative electrode material, including following step
It is rapid:
1) with one of needle coke, pitch coke coke powder for raw material, fugitive constituent≤8% of the raw material, coke powder partial size: D
≤1mm；
2) it crushes: being crushed needle coke with airslide disintegrating mill, D50 is at 8~18 μm；
3) it is graphitized: 2800~3000 DEG C of graphitization temperature, obtaining graphous graphite powder；
4) it coats: graphous graphite powder and high softening point bitumen powder that previous step obtains being added in coating reaction kettle and mixed
Cladding；High softening point bitumen property: QI≤0.1%, softening point: 250~270 DEG C, D50:4~8 μm；High softening point bitumen is added
Measure 3%~15wt%, 85%~97wt% of graphite powder additional amount；Temperature of plate: 270~300 DEG C, 1~2h of time is coated；
5) mixture coated is carbonized under 700-1000 DEG C of temperature, nitrogen atmosphere 1-3h, is sieved after being cooled to room temperature,
Finally prepare high performance lithium ion battery negative material.
It is required that it is the value in order to improve needle coke coke breeze that raw material particle size, which is less than 1mm, while negative electrode material raw material can be reduced
Cost.
The method of solid asphalt low temperature cladding preparation negative electrode material according to the present invention, it is preferred that described in step 4)
Coating reaction kettle is the reaction kettle of the double ribbon agitating paddles of band.
The method of solid asphalt low temperature cladding preparation negative electrode material according to the present invention, it is preferred that the step 5) charcoal
The change time is 0.5-2h.
The method of solid asphalt low temperature cladding preparation negative electrode material according to the present invention, it is preferred that the lithium-ion electric
Take off for the first time lithium capacity (0.2C) that button cell is made in pond negative electrode material is 350-360mAh/g.
The method of solid asphalt low temperature cladding preparation negative electrode material according to the present invention, it is preferred that the lithium-ion electric
The coulombic efficiency for the first time of button cell is made up to 92% or more in pond negative electrode material.
The present invention is to coat one layer of pitch on graphite material (needle coke, pitch coke) surface, in graphite surface after carbonizing
As soon as forming a layer amorphous carbon, a kind of " core-shell structure copolymer " structure is formed with the graphite of the inside cladding in this way.This structure is conducive to reduce lithium
The loss of ion, while the coulombic efficiency for the first time of charge and discharge can also be greatly improved.
The negative electrode material is made into button cell, and chemical property detection is carried out to the button cell.The result shows that adopting
The negative electrode material made of the art of this patent has excellent chemical property, and specific effect see the table below:
The cathode material chemical property of 1 this technology of table preparation
The utility model has the advantages that
The present invention relates to one kind to prepare high-quality artificial graphite by the modification of solid asphalt low temperature clad surface with calcined coke powder
The technology of Li-like ions cell negative electrode material, specially forge rear needle coke coke powder, pitch coke coke powder etc. with partial size less than 1mm are
Raw material is graphitized after airslide disintegrating mill is crushed to certain partial size, is then carried out surface and is modified, that is, uses solid high softening-point
Pitch coats artificial graphite aggregate under cryogenic, handles using high temperature carbonization, and pitch is made to decompose polycondensation
Reaction forms the negative electrode material of the function admirable of " core-shell structure copolymer " structure.Needle coke, pitch coke are to prepare graphite electrode, special charcoal respectively
Raw material, and partial size less than 1mm forge rear needle coke coke powder, pitch coke coke powder be graphite electrode, Te Tan producer it is undesired or
It is used for degrading, therefore, needle coke coke powder, pitch coke coke powder are cheap.Meanwhile needle coke coke powder, pitch coke coke powder have
There is poor fibre structure, is the raw material of preferable negative electrode material.With forge rear needle coke coke powder, pitch coke coke powder prepare lithium electricity
Pond negative electrode material can not only reduce cost of material, but also be able to ascend the performance of lithium cell cathode material.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Embodiment 1: D50:14.8 μm of needle-shaped coke powder, volatile matter: 6.0%；3000 DEG C of graphitization temperature, high softening point bitumen
D50:6 μm of powder, QI:0.05%, softening point: 258 DEG C；Needle-shaped coke powder: high softening point bitumen powder=4%:96%；Temperature of plate
280 DEG C, coat time 2h；Carbonization temperature: 900 DEG C, carbonization time: 1h.Button is assembled into negative electrode material prepared by the technology
Battery, taking off lithium capacity for the first time is 355.6mAh/g, and coulomb effect is 95.6% for the first time, and detaining electric multiplying power (1C/0.2C) is 50.5%.
Embodiment 2: D50:16.5 μm of needle-shaped coke powder, volatile matter: 5.1%；3000 DEG C of graphitization temperature, high softening point bitumen
D50:8 μm of powder, QI:0.05%, softening point: 258 DEG C；Needle-shaped coke powder: high softening point bitumen powder=6%:94%；Temperature of plate
290 DEG C, coat time 1.5h；Carbonization temperature: 1000 DEG C, carbonization time: 1h.Button is assembled into negative electrode material prepared by the technology
Formula battery, taking off lithium capacity for the first time is 354.8mAh/g, and coulomb effect is 94.6% for the first time, detains electric multiplying power (1C/0.2C) and is
47.8%.
Embodiment 3: D50:15.3 μm of needle-shaped coke powder, volatile matter: 7.1%；3000 DEG C of graphitization temperature, high softening point bitumen
D50:7 μm of powder, QI:0.05%, softening point: 258 DEG C；Needle-shaped coke powder: high softening point bitumen powder=7%:93%；Temperature of plate
280 DEG C, coat time 2h；Carbonization temperature: 950 DEG C, carbonization time: 1h.Button is assembled into negative electrode material prepared by the technology
Battery, taking off lithium capacity for the first time is 353.6mAh/g, and coulomb effect is 93.5% for the first time, and detaining electric multiplying power (1C/0.2C) is 48.5%.
Embodiment 4: D50:14.8 μm of pitch coke coke powder, volatile matter: 6.0%；3000 DEG C of graphitization temperature, high softening-point drip
D50:8 μm, QI:0.05% of green powder, softening point: 258 DEG C；Pitch coke coke powder: high softening point bitumen powder=5%:95%；Cladding temperature
280 DEG C of degree coats time 2h；Carbonization temperature: 1000 DEG C, carbonization time: 1h.Button is assembled into negative electrode material prepared by the technology
Formula battery, taking off lithium capacity for the first time is 350.1mAh/g, and coulomb effect is 92.3% for the first time, detains electric multiplying power (1C/0.2C) and is
46.8%.
The present invention forges rear needle coke, pitch coke coke powder as raw material less than 1mm using partial size, is crushed to one through airslide disintegrating mill
It is graphitized after determining partial size, coke powder and high softening point bitumen powder are added in cladding kettle and carry out low temperature packet after being then graphitized
It covers, so that artificial graphite surface is uniformly coated one layer of pitch, handled using high temperature carbonization, make pitch that thermal polycondensation reaction occur,
Form the negative electrode material of the function admirable of " core-shell structure copolymer " structure.
The present invention uses the method for coating, carbonizing again that is first graphitized, and at low temperature (less than 300 DEG C), and coats the time
Only need 1~2 hour.The negative electrode material of preparation takes off lithium capacity for the first time, and coulombic efficiency is more than 350mAh/g for the first time, for the first time coulombic efficiency
Reachable 92% or more, superior performance.Therefore, the negative electrode material simple process prepared with this method, production cost is low and has height
Performance.
Claims (5)
1. a kind of method of solid asphalt low temperature cladding preparation negative electrode material, it is characterised in that: the following steps are included:
1) with one of needle coke, pitch coke coke powder for raw material, fugitive constituent≤8% of the raw material, coke powder partial size: D≤
1mm；
2) it crushes: being crushed needle coke with airslide disintegrating mill, D50 is at 8~18 μm；
3) it is graphitized: 2800~3000 DEG C of graphitization temperature, obtaining graphous graphite powder；
4) coat: the graphous graphite powder and high softening point bitumen powder that previous step is obtained, which are added in coating reaction kettle, mixes packet
It covers；High softening point bitumen property: QI≤0.1%, softening point: 250~270 DEG C, D50:4~8 μm；High softening point bitumen additional amount
3%~15wt%, 85%~97wt% of graphite powder additional amount；Temperature of plate: 270~300 DEG C, 1~2h of time is coated；
5) mixture coated is carbonized under 700-1000 DEG C of temperature, nitrogen atmosphere 1-3h, be sieved after being cooled to room temperature, finally
Prepare high performance lithium ion battery negative material.
2. the method for solid asphalt low temperature cladding preparation negative electrode material according to claim 1, it is characterised in that: step 4)
The coating reaction kettle is the reaction kettle of the double ribbon agitating paddles of band.
3. the method for solid asphalt low temperature cladding preparation negative electrode material according to claim 1, it is characterised in that: step 5)
The carbonization time is 0.5-2h.
4. the method for solid asphalt low temperature cladding preparation negative electrode material according to claim 1, it is characterised in that: the lithium
Take off for the first time lithium capacity (0.2C) that button cell is made in ion battery cathode material is 350-360mAh/g.
5. the method for solid asphalt low temperature cladding preparation negative electrode material according to claim 1, it is characterised in that: the lithium
The coulombic efficiency for the first time of button cell is made up to 92% or more in ion battery cathode material.
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Cited By (12)
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| CN112133894A (en) * | 2020-09-03 | 2020-12-25 | 深圳石墨烯创新中心有限公司 | Negative electrode material for lithium battery and preparation method of material |
| CN112382794A (en) * | 2020-08-03 | 2021-02-19 | 万向一二三股份公司 | Preparation method of graphite cathode lithium ion battery |
| CN112661148A (en) * | 2020-12-24 | 2021-04-16 | 宁波杉杉新材料科技有限公司 | Composite graphite negative electrode material, preparation method and application thereof, and lithium ion battery |
| CN112794321A (en) * | 2021-01-15 | 2021-05-14 | 中国神华煤制油化工有限公司 | Carbon negative electrode material and preparation method and application thereof |
| CN112938960A (en) * | 2021-01-29 | 2021-06-11 | 乌海宝杰新能源材料有限公司 | Preparation method of high-compaction-density and low-specific-surface-area negative electrode material |
| CN113101887A (en) * | 2021-04-22 | 2021-07-13 | 湖南阿斯米科技有限公司 | Graphite type cathode material/phosphate and ternary cathode material continuous reaction treatment equipment for lithium ion battery |
| CN113258063A (en) * | 2021-04-29 | 2021-08-13 | 河南易成瀚博能源科技有限公司 | Method for preparing graphite cathode material of lithium ion battery by spray drying method |
| CN114804877A (en) * | 2022-05-19 | 2022-07-29 | 李鑫 | Pulse current internal heating type intermediate temperature graphitized negative electrode material and manufacturing method thereof |
| CN114804062A (en) * | 2021-01-18 | 2022-07-29 | 宝武碳业科技股份有限公司 | Coke for lithium ion battery cathode material and preparation method thereof |
| CN115806290A (en) * | 2022-12-06 | 2023-03-17 | 广东凯金新能源科技股份有限公司 | Artificial graphite lithium ion battery cathode material and preparation method thereof |
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| CN114804877A (en) * | 2022-05-19 | 2022-07-29 | 李鑫 | Pulse current internal heating type intermediate temperature graphitized negative electrode material and manufacturing method thereof |
| CN114804877B (en) * | 2022-05-19 | 2024-01-23 | 深圳市钢昱碳晶科技有限公司 | Pulse current internal heating type medium-temperature graphitized anode material and manufacturing method thereof |
| CN115893400A (en) * | 2022-11-15 | 2023-04-04 | 晖阳(贵州)新能源材料有限公司 | Preparation method of negative electrode material for long-cycle lithium ion battery |
| CN115893400B (en) * | 2022-11-15 | 2023-10-10 | 贵州晖阳科技创新研究有限公司 | Preparation method of negative electrode material for long-cycle lithium ion battery |
| CN115806290A (en) * | 2022-12-06 | 2023-03-17 | 广东凯金新能源科技股份有限公司 | Artificial graphite lithium ion battery cathode material and preparation method thereof |
| CN115806290B (en) * | 2022-12-06 | 2024-08-13 | 广东凯金新能源科技股份有限公司 | Artificial graphite lithium ion battery negative electrode material and preparation method thereof |
| CN116443869A (en) * | 2023-03-17 | 2023-07-18 | 乌海宝杰新能源材料有限公司 | Quick graphite charging negative electrode material for starting and stopping power supply and preparation method thereof |
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