CN110289417A - A kind of artificial graphite cathode material for lithium ion batteries preparation method - Google Patents
A kind of artificial graphite cathode material for lithium ion batteries preparation method Download PDFInfo
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- CN110289417A CN110289417A CN201910558490.XA CN201910558490A CN110289417A CN 110289417 A CN110289417 A CN 110289417A CN 201910558490 A CN201910558490 A CN 201910558490A CN 110289417 A CN110289417 A CN 110289417A
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- lithium ion
- petroleum coke
- ion batteries
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/205—Preparation
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- 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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Abstract
The invention discloses a kind of artificial graphite cathode material for lithium ion batteries preparation methods, using petroleum coke and coal tar as raw material, polymerization reaction is carried out at a temperature of 300 ~ 600 DEG C, with 5 ~ 20 μm of powdered carbon of partial size, graphitization heat treatment is directly over and forms artificial plumbago negative pole material.The present invention has the advantages that low temperature properties good (be suitble to the north cold weather), high magnification, having extended cycle life, it is suitable for digital and power lithium battery.
Description
Technical field
The present invention relates to a kind of technical field of lithium ion battery negative, especially a kind of lithium ion battery artificial graphite
Cathode material preparation method.
Background technique
Currently, lithium ion battery as a kind of rechargeable battery, has, operating voltage is high, performance is stable, discharge potential is bent
Line is steady, self discharge is small, have extended cycle life, low temperature performance well, environmental protection, it is memoryless the advantages that.The preparation of lithium ion battery is crucial
One of technology is the selection and research of negative electrode material, and the quality of negative electrode material directly affects the electrochemistry of battery
Energy.
Graphite negative electrodes material has many advantages, such as that cycle efficieny is high, cycle performance is good, resourceful, cheap, and
As ideal lithium ion battery negative material.But graphite type material has layer structure or sclay texture, graphite linings more
Between with weaker combination, the insertion of solvation lithium ion and the total insertion of solvent molecule, layer and layer are be easy to cause in charge and discharge
Between can generate removing and form new surface, organic electrolyte continuous reduction decomposition on the surface newly formed forms new
SEI film had both consumed a large amount of lithium ion, increased irreversible capacity loss for the first time, and due to the insertion of solvation lithium ion and
Abjection causes the volume expansion and contraction of graphite particle, and intergranular energization network portion is caused to interrupt, to occur because of graphite
The distinctive layer structure of class material or sclay texture and influence its stability, cycle performance and security performance.Lithium ion secondary
The negative electrode material of battery is presently mainly graphite microparticles.Wherein, common graphous graphite powder is in irregular shape, and large specific surface area is led
Material poor processability is caused, chemical property is weaker.
Therefore lithium ion battery new material is explored to emerge one after another.According to 106654269 B of Chinese patent Authorization Notice No. CN,
" a kind of graphite cathode material and its preparation method and application for power lithium-ion battery is disclosed, method includes: by carbon materials
Material is uniformly mixed with asphalt powder by the weight ratio of 100:0.1~25, is granulated, is obtained granulation material；Granulation material is subjected to broken classification
Processing, obtains shaping material；Shaping material is uniformly mixed with pitch by 100:0~10, is carried out at graphitization at 2000~3300 DEG C
Reason, the graphite material purified；The graphite material and polymer powder of purification are uniformly dispersed in the water containing CMC-Na,
The suspension of formation is spray-dried；Wherein, graphite material and the weight ratio of polymer powder are 100:1~10, CMC-
Na weight ratio is 100:0.5~3；It in 1000~1300 DEG C of progress carbonization treatments, is sieved after cooling and obtains graphite cathode material ".
It can satisfy high magnification fast electric so exploring a kind of new method to prepare, while having both the graphite cathode of high capacity
Material be very it is necessary to.
All there is cannot effectively improve artificial graphite class battery cathode material for above-mentioned various improved methods reported in the literature.
Expect the low deficiency of the compacted density problem low with discharge capacity.
Summary of the invention
Present invention problem in view of the prior art, provides a kind of artificial graphite cathode material for lithium ion batteries preparation side
Negative electrode material production cost is effectively reduced to reach simple process, high-efficient, low temperature performance well in method, improves discharge-rate, makes
The material circulation service life is long.
The present invention is realized using such method: a kind of artificial graphite cathode material for lithium ion batteries preparation method,
Include the following steps: step 1, selects petroleum coke and coal tar is step 2 raw material is dried, step 3, with shearing crushing
Machine crushes petroleum coke and step 4 accounts for 5,8,11,15,18% number ratio, petroleum coke and coal tar in petroleum coke to 5-20 μm of granularities
Oil carries out polymerization reaction at a temperature of 300-600 DEG C, realizes cladding, granulation, petroleum coke particles and coal tar during the reaction
Polymerization terminates reaction when 600 DEG C, and total reaction time is 6 hours, and the product for forming reaction is in flow regime, step 5, warp
It is put into packing material after second level kettle is cooling；Step 6, through dismiss machine continuous-flow type dismiss, step 7, after go to 2900-3000 DEG C of temperature
Degree is lower to carry out graphitization processing, and the processing reaction time is 48 hours, step 8, uniformly mixes through mixing machine, step 9, through dry type electricity
Magnetic magneticly elects metallic foreign body except magnetomechanical, and step 10, through ultrasonic screening machine, 375 mesh screens filter out unqualified foreign matter, step
11, step 12 packaging, eventually forms artificial plumbago negative pole material.
Further, preferably, the pulverizer is shearing crusher.
Further, preferably, the heat treatment polymerization equipment is that double helical-ribbon types heat reaction kettle.
Further, preferably, the graphitization equipment is acheson furnace.
Further, preferably, petroleum coke is 2#A low sulfur petroleum coke NB/SH/T 05272015.
Further, preferably, coal tar is oily mixture YB/T 5075-93 obtained from the dry distillation of coal.
It illustrates, what above-mentioned all numbers referred to is all parts by weight.
The beneficial effects of the present invention are:
1, simple production process of the present invention, high-efficient, low temperature performance well, are effectively reduced negative electrode material production cost.
2, it is adjusted according to the grain shape of petroleum coke, improves the surface density of negative pole piece of battery, effectively improve electric discharge times
Rate keeps the material circulation service life long.
3, the present invention sets the ratio of different cladding coal tar, makes artificial plumbago negative pole material according to raw material granularity difference
Electrical property most preferably played.
The main performance index of 1 artificial plumbago negative pole material of table
18 ± 1 μm of granularity (D50)
Real density >=2.24 g/cm3
Ash content≤0.05
2.0 ± 0.3 m of specific surface area2/g
1.0 ± 0.1 g/cm of tap density3
Moisture≤0.10
Thermal bounce≤10%
350 ± 5 mAh/g of discharge capacity for the first time
Discharging efficiency 92% -95% for the first time.
Detailed description of the invention
What Fig. 1 was provided is process flow diagram of the invention
Below with reference to Fig. 1, the present invention is further illustrated, but the present invention is not limited to these Examples.
Specific embodiment
Embodiment 1
As shown in Figure 1: a kind of artificial graphite cathode material for lithium ion batteries preparation method includes the following steps: step 1, selects
Petroleum coke and coal tar are step 2 raw material is dried, and step 3, crush petroleum coke to 5-20 μm of grains with shearing crusher
Degree, step 4, accounts for 5,8,11,15,18% number ratio in petroleum coke, petroleum coke and coal tar carry out at a temperature of 300-600 DEG C
Polymerization reaction realizes that cladding, granulation, petroleum coke particles polymerize with coal tar during the reaction, reaction is terminated when 600 DEG C,
Total reaction time is 6 hours, and the product for forming reaction is in flow regime, step 5, is put into packing material after second level kettle is cooling
It is interior；Step 6, through dismiss machine continuous-flow type dismiss, step 7, after go to 2900-3000 DEG C at a temperature of carry out graphitization processing, handle
Reaction time is 48 hours, step 8, is uniformly mixed through mixing machine, step 9, through dry type electromagnetism except magnetomechanical magneticly elects metallic foreign body,
Step 10, through ultrasonic screening machine, 375 mesh screens filter out unqualified foreign matter, and step 11, step 12 packaging, eventually forms
Artificial plumbago negative pole material product.
Further, preferably, the pulverizer is shearing crusher.
Further, preferably, the heat treatment polymerization equipment is that double helical-ribbon types heat reaction kettle.
Further, preferably, the graphitization equipment is acheson furnace.
Further, preferably, petroleum coke is 2#A low sulfur petroleum coke NB/SH/T 05272015.
Further, preferably, coal tar is oily mixture YB/T 5075-93 obtained from the dry distillation of coal.
Embodiment 2
Raw material granularity D50 is set as 5 μm, sets the ratio of different cladding coal tar, makes the electrical property of artificial plumbago negative pole material
It is most preferably played, accounts for 5,8,11,15,18% number ratio in petroleum coke.
Embodiment 3
Raw material granularity D50 is set as 7 μm, sets the ratio of different cladding coal tar, makes the electrical property of artificial plumbago negative pole material
It is most preferably played, accounts for 5,8,11,15,18% number ratio in petroleum coke.
Embodiment 4
Raw material granularity D50 is set as 9 μm, sets the ratio of different cladding coal tar, makes the electrical property of artificial plumbago negative pole material
It is most preferably played, accounts for 5,8,11,15,18% number ratio in petroleum coke.
Embodiment 5
Raw material granularity D50 is set as 11 μm, sets the ratio of different cladding coal tar, makes the electrical property of artificial plumbago negative pole material
It is most preferably played, accounts for 5,8,11,15,18% number ratio in petroleum coke.
Embodiment 6
Raw material granularity D50 is set as 18 μm, sets the ratio of different cladding coal tar, makes the electrical property of artificial plumbago negative pole material
It is most preferably played, accounts for 5,8,11,15,18% number ratio in petroleum coke.
Claims (6)
1. a kind of artificial graphite cathode material for lithium ion batteries preparation method, characterized by the following steps: step 1, choosing
It is raw material with petroleum coke and coal tar, step 2, is dried, step 3, crushes petroleum coke to 5 ~ 20 μm with shearing crusher
Granularity, step 4, in petroleum coke account for 5,8,11,15,18% number ratio, petroleum coke and coal tar at a temperature of 300 ~ 600 DEG C into
Row polymerization reaction is realized that cladding, granulation, petroleum coke particles polymerize with coal tar during the reaction, is terminated when 600 DEG C anti-
It answers, total reaction time is 6 hours, and the product for forming reaction is in flow regime, step 5, is put into packaging after second level kettle is cooling
In object；Step 6, through dismiss machine continuous-flow type dismiss, step 7, after go to 2900 ~ 3000 DEG C at a temperature of carry out graphitization processing, locate
Managing the reaction time is 48 hours, step 8, is uniformly mixed through mixing machine, step 9, different except magnetomechanical magneticly elects metal through dry type electromagnetism
Object, step 10, through ultrasonic screening machine, 375 mesh screens filter out unqualified foreign matter, step 11, packaging, and step 12, last shape
At artificial plumbago negative pole material.
2. a kind of artificial graphite cathode material for lithium ion batteries preparation method according to claim 1, it is characterised in that: institute
The pulverizer stated is shearing crusher.
3. a kind of artificial graphite cathode material for lithium ion batteries preparation method according to claim 1, it is characterised in that: institute
The heat treatment polymerization equipment stated is that double helical-ribbon types heat reaction kettle.
4. a kind of artificial graphite cathode material for lithium ion batteries preparation method according to claim 1, it is characterised in that: institute
The graphitization equipment stated is acheson furnace.
5. a kind of artificial graphite cathode material for lithium ion batteries preparation method according to claim 1, it is characterised in that: stone
Oil coke is 2#A low sulfur petroleum coke NB/SH/T 05272015.
6. a kind of artificial graphite cathode material for lithium ion batteries preparation method according to claim 1, it is characterised in that: coal
Tar is oily mixture YB/T 5075 obtained from the dry distillation of coal.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114512652A (en) * | 2022-02-22 | 2022-05-17 | 新疆天宏基科技有限公司 | Process for reducing specific surface area of graphite negative electrode material of lithium battery |
| EP4043397A4 (en) * | 2020-01-10 | 2023-01-25 | LG Energy Solution, Ltd. | Artificial graphite, method for preparing artificial graphite, anode comprising same, and lithium secondary battery |
| CN115872398A (en) * | 2022-12-05 | 2023-03-31 | 重庆东星炭素材料有限公司 | Single particle anode material for producing medium sulfur coke |
| CN117550593A (en) * | 2024-01-11 | 2024-02-13 | 上海巴库斯超导新材料有限公司 | Novel preparation process of natural graphite anode material |
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| CN106495144A (en) * | 2015-11-17 | 2017-03-15 | 宁波杉杉新材料科技有限公司 | A kind of low bulk long circulating Delanium lithium ion battery negative material |
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| CN104659365A (en) * | 2014-12-30 | 2015-05-27 | 东莞市凯金新能源科技有限公司 | Preparation method of artificial graphite anode material for lithium ion battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4043397A4 (en) * | 2020-01-10 | 2023-01-25 | LG Energy Solution, Ltd. | Artificial graphite, method for preparing artificial graphite, anode comprising same, and lithium secondary battery |
| CN114512652A (en) * | 2022-02-22 | 2022-05-17 | 新疆天宏基科技有限公司 | Process for reducing specific surface area of graphite negative electrode material of lithium battery |
| CN114512652B (en) * | 2022-02-22 | 2024-04-26 | 新疆天宏基科技有限公司 | Process for reducing specific surface area of graphite cathode material of lithium battery |
| CN115872398A (en) * | 2022-12-05 | 2023-03-31 | 重庆东星炭素材料有限公司 | Single particle anode material for producing medium sulfur coke |
| CN117550593A (en) * | 2024-01-11 | 2024-02-13 | 上海巴库斯超导新材料有限公司 | Novel preparation process of natural graphite anode material |
| CN117550593B (en) * | 2024-01-11 | 2024-04-26 | 上海巴库斯超导新材料有限公司 | Novel preparation process of natural graphite anode material |
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Inventor after: Ding Desheng Inventor after: Wang Fuzhi Inventor before: Ding Desheng |