CN106532050A - Lithium ion battery high capacity hard carbon cathode material and preparation method thereof - Google Patents
Lithium ion battery high capacity hard carbon cathode material and preparation method thereof Download PDFInfo
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- CN106532050A CN106532050A CN201510581373.7A CN201510581373A CN106532050A CN 106532050 A CN106532050 A CN 106532050A CN 201510581373 A CN201510581373 A CN 201510581373A CN 106532050 A CN106532050 A CN 106532050A
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- hard carbon
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- lithium ion
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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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- 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
Abstract
The invention discloses a lithium ion battery high capacity hard carbon cathode material and a preparation method thereof. The method comprises the following steps: (1) a polymerization reaction is carried out for an organic matter and alkenyl aromatic hydrocarbons, in order to obtain a polymer; (2) solvent extraction processing is carried out for the polymer at 50-100 DEG C for 2-6 hours; (3) vacuum drying treatment is carried out, the temperature is reduced to the room temperature, and the materials are crushed and sieved; (3) under protection of inert gas, pre-carbonization is carried out at 300-650 DEG C and low temperature thermal refining is carried out, the temperature is cooled to the room temperature, and crushing and screening are carried out; (5) under the protection of inert gas, high temperature carbonization treatment is carried out at 900-1900 DEG C, and the material is obtained. The first discharge capacity of the lithium ion battery high capacity hard carbon cathode material is above 450mAh/g, and the first charge-discharge efficiency is above 90%. The preparation method is simple and easy to operate, and raw material sources are wide and cost is low.
Description
Technical field
The present invention relates to field of batteries, the lithium ion that specifically a kind of organic matter is obtained through polymerisation and high temperature carbonization process
The preparation method of cell high-capacity hard carbon cathode material and high power capacity hard carbon cathode material obtained by this method.
Background technology
Into 21 century, with petroleum reserves increasingly depleted on the earth, and the greenhouse that motor vehicle exhaust emission is produced to environment
Effect, in recent years, as new application the features such as effectively utilizes lithium ion battery small volume light weight, is energetically carried out
As only using the hybrid electric automobile (HEV) of the electric automobile (EV) of motor-driven, engine and motor combination
The exploitation of these batteries used for electric vehicle, wherein, EV/PHEV has higher-energy power density and longer cruising time
Feature.
Hard carbon cathode material due to the macromolecular deck structure of its firm stable, it is preferably under high current charge-discharge use and it is standby
Concerned, its good security performance is expected to be applied on electric automobile.So, for PHEV/EV is dynamic with lithium ion
Power battery, it is desirable to the characteristic different from existing small-sized Portable device purposes.
Japan Patent CN1947286A prepares difficult graphitization carbon with the oxidation of porous pelletted pitch fluid bed, charing method,
This method has complicated process of preparation, manufactures cost high-leveled and difficult in realization commercialization.Chinese patent CN1191195C be by
Liquid-phase dehydration, the washing in the autoclave such as resin are dried the hard carbon material of high temperature carbonization preparation, equally exist preparation technology loaded down with trivial details
It is difficult to the problems such as realizing industrialized production.
The content of the invention
It is an object of the invention to provide a kind of easy lithium ion cell high-capacity hard carbon cathode material of simple process and its system
Preparation Method, to solve the problems, such as to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme：
A kind of preparation method of lithium ion cell high-capacity hard carbon cathode material, which comprises the steps：1. by organic matter and alkene
Base aromatic hydrocarbons carries out polymerisation, obtains polymer；2. polymer is carried out solvent extraction to process 2～6 hours at 50～100 DEG C；
3. vacuum drying treatment, is cooled to room temperature, crushes and screens；4., under inert gas shielding, carbonized in 300～650 DEG C in advance low
Warm modifier treatment, is cooled to room temperature, crushes and screens；5. under inert gas shielding, at 900～1900 DEG C of high temperature carbonizations
Reason is obtained final product.
As further scheme of the invention：Step 1. in, organic matter be naphthalene, anthracene, phenanthrene, epoxy resin or phenolic resin.
As further scheme of the invention：Alkenyl arene of the alkenyl arene for carbon atom 8～10.
As further scheme of the invention：Polymerization reaction time is 1～15 hour；Polymeric reaction temperature is 50～300 DEG C.
Step 1. in organic matter carry out polymerisation, it is therefore an objective to by organic matter formed macromolecular plane mesh structure, improve material big
Current charge-discharge electrical property.
As further scheme of the invention：Step 2. in, solvent be washing oil, quinoline, toluene, the one kind in dimethylbenzene with
On mixture.
As further scheme of the invention：Step 3. in vacuum drying treatment adopt vacuum drying chamber, step 4. in it is pre-
Charing low temperature modifier treatment adopts well formula retort, step 5. in high temperature carbonization process using pushed bat kiln high temperature carbonization furnace.
Lithium ion battery negative material is obtained by above-mentioned preparation method, its first discharge capacity it is in more than 450mAh/g, first
Secondary efficiency for charge-discharge is more than 90%.
Compared with prior art, the invention has the beneficial effects as follows：
Problem present in current material preparation process can be efficiently solved by the preparation method of the present invention, described hard carbon is born
Pole material is a kind of carbon negative pole material of organic matter through polymerisation, solvent extraction process and charing process.Polymerization therein
Reaction, solvent extraction process and charing process process are simple and easy to do, and raw material sources are extensively and low cost.Due to have passed through
The methods such as polymerisation, high temperature carbonization process and crushing and classification, cause obtained product capacity to play and good cycle, its
Performance parameter is as shown in table 1 below.
Table 1
The high power capacity hard carbon cathode material of the present invention, the high comprehensive performance of button cell made by which mainly have the advantage that：
1. chemical property is good, and, in more than 450mAh/g, first charge-discharge efficiency is more than 90% for discharge capacity；2. high current is filled
Discharge performance is preferable；3. good cycle (5000 circulations, capability retention >=80%)；4. security is preferable (130 DEG C
/ 60 minutes, it is not quick-fried, do not rise)；5. it is preferable to electrolyte and other additive adaptability；6. product property is stable, batch
Between almost no difference.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of hard carbon cathode material of the present invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, is shown
So, described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.Based in the present invention
Embodiment, the every other embodiment obtained under the premise of creative work is not made by those of ordinary skill in the art, all
Belong to the scope of protection of the invention.
Raw material in following examples is conventional commercial product.
Embodiment 1
Divinylbenzene 200g, hydrochloric acid 100g and naphthalene 1000g are added in reactor under stirring and are mixed, be warming up to 180 DEG C
Polymerisation 8 hours, reaction are cooled to 100 DEG C of washing oil solvents and process 2 hours after terminating, heat filtering, filter cake vacuum (- 0.09～
- 0.1MPa, 150 DEG C) it is dried 2 hours, room temperature discharging is down to, crushed material is crossed into 100 eye mesh screens after crushing, load well formula
In retort, being warming up to 500 DEG C under nitrogen protection carries out pre- charing process 5 hours, is cooled to room temperature, by powder after crushing
Minced 100 eye mesh screens, in 1400 DEG C of charing process 5 hours in pushed bat kiln under nitrogen protection, hard carbon cathode material is obtained
Material, discharge capacity is 450.6mAh/g to its half-cell first, first discharging efficiency 91.2%.
Embodiment 2
Divinylbenzene 300g, hydrochloric acid 100g and naphthalene 1000g are added in reactor under stirring and are mixed, be warming up to 180 DEG C
Polymerisation 8 hours, reaction are cooled to 50 DEG C of toluene solvants and process 6 hours after terminating, heat filtering, filter cake vacuum (- 0.09～
- 0.1MPa, 150 DEG C) it is dried 2 hours, crushed material is crossed into 100 eye mesh screens after crushing, loads well formula retort, in nitrogen
Being warming up to 500 DEG C under protection carries out pre- charing process 5 hours, is cooled to room temperature, and crushed material is crossed 100 eye mesh screens after crushing,
In 1900 DEG C of charing process 3 hours in pushed bat kiln under nitrogen protection, hard carbon cathode material is obtained, its half-cell is put first
Capacitance is 456.4mAh/g, first discharging efficiency 91.5%.
Embodiment 3
Trivinylbenzene 200g, hydrochloric acid 200g and anthracene 1000g are alternately added in reactor under stirring and are mixed, be warming up to
180 DEG C of polymerisations 8 hours, reaction are cooled to 80 DEG C of xylene solvents and process 4 hours after terminating, heat filtering, filter cake are true
Empty (- 0.09～-0.1MPa, 150 DEG C) is dried 2 hours, is down to room temperature discharging, crushed material is crossed 100 mesh sieves after crushing
Net, loads well formula retort, and being warming up to 500 DEG C under nitrogen protection carries out pre- charing process 5 hours, is cooled to room temperature,
Crushed material is crossed into 100 eye mesh screens after crushing, in 1400 DEG C of charing process 5 hours in pushed bat kiln under nitrogen protection, is obtained
Hard carbon cathode material, discharge capacity is 455.7mAh/g to its half-cell first, first discharging efficiency 90.5%.
Embodiment 4
Divinylbenzene 300g, nitric acid 200g and naphthalene 1000g are added in reactor under stirring and are mixed, be warming up to 180 DEG C
Polymerisation 8 hours, reaction terminate rear temperature and process 2 hours in 100 DEG C of washing oil solvents, heat filtering, filter cake vacuum (- 0.09～
- 0.1MPa, 150 DEG C) it is dried 2 hours, room temperature discharging is down to, crushed material is crossed into 100 eye mesh screens after crushing, load well formula
Retort, being warming up to 500 DEG C under nitrogen protection carries out pre- charing process 5 hours, is cooled to room temperature, will crush after crushing
Thing crosses 100 eye mesh screens, in 1400 DEG C of charing process 5 hours in pushed bat kiln under nitrogen protection, hard carbon cathode material is obtained,
Discharge capacity is 457.1mAh/g to its half-cell first, first discharging efficiency 90.5%.
Embodiment 5
Divinylbenzene 500g, hydrochloric acid 150g and phenolic resin 1000g are added in reactor under stirring and are mixed, heated up
To 180 DEG C of polymerisations 8 hours, reaction terminated rear temperature and processes 2 hours in 100 DEG C of washing oil solvents, heat filtering, filter cake
Vacuum (- 0.09～-0.1MPa, 150 DEG C) is dried 2 hours, is down to room temperature discharging, crushed material is crossed 100 mesh after crushing
Screen cloth, loads well formula retort, and being warming up to 500 DEG C under nitrogen protection carries out pre- charing process 5 hours, is cooled to room temperature,
Crushed material is crossed into 100 eye mesh screens after crushing, in 1400 DEG C of charing process 5 hours in pushed bat kiln under nitrogen protection, is obtained
Hard carbon cathode material, discharge capacity is 454.3mAh/g to its half-cell first, first discharging efficiency 90.7%.
Embodiment 6
Divinylbenzene 200g, hydrochloric acid 100g and epoxy resin 1000g are added in reactor under stirring and are mixed, heated up
To 50 DEG C of polymerisations 15 hours, reaction was cooled to 50 DEG C of quinoline solvents and processes 2 hours after terminating, heat filtering, filter cake are true
Empty (- 0.09～-0.1MPa, 150 DEG C) is dried 2 hours, is down to room temperature discharging, crushed material is crossed 100 mesh sieves after crushing
Net, loads well formula retort, and being warming up to 500 DEG C under nitrogen protection carries out pre- charing process 1 hour, is cooled to room temperature,
Crushed material is crossed into 100 eye mesh screens after crushing, in 1400 DEG C of charing process 5 hours in pushed bat kiln under nitrogen protection, is obtained
Hard carbon cathode material, discharge capacity is 451.5mAh/g to its half-cell first, first discharging efficiency 90.8%.
Embodiment 7
Divinylbenzene 300g, hydrochloric acid 200g and naphthalene 1000g are alternately added in reactor under stirring and are mixed, be warming up to
180 DEG C of polymerisations 8 hours, reaction terminate rear temperature and process 2 hours in 80 DEG C of washing oil toluene Mixed Solvents, heat filtering,
Filter cake vacuum (- 0.09～-0.1MPa, 150 DEG C) is dried 2 hours, is down to room temperature discharging, crushed material is crossed 100 after crushing
Eye mesh screen, loads well formula retort, and being warming up to 300 DEG C under nitrogen protection carries out pre- charing process 10 hours, is cooled to room
Crushed material is crossed 100 eye mesh screens after crushing by temperature, in 900 DEG C of charing process 10 hours in pushed bat kiln under nitrogen protection,
Prepared hard carbon cathode material, discharge capacity is 460.1mAh/g to its half-cell first, first discharging efficiency 90.7%.
Embodiment 8
Divinylbenzene 200g, hydrochloric acid 200g and naphthalene 1000g are alternately added in reactor under stirring and are mixed, be warming up to
300 DEG C of polymerisations 1 hour, reaction terminate rear temperature and process 4 hours in 80 DEG C of washing oil solvents, heat filtering, filter cake vacuum
(- 0.09～-0.1MPa, 150 DEG C) is dried 2 hours, is down to room temperature discharging, crushed material is crossed 100 eye mesh screens after crushing,
Load well formula retort, being warming up to 650 DEG C under nitrogen protection carries out pre- charing process 5 hours, is cooled to room temperature, crush
Crushed material is crossed into 100 eye mesh screens afterwards, in 1400 DEG C of charing process 1 hour in pushed bat kiln under nitrogen protection, hard carbon is obtained
Negative material, discharge capacity is 454.3mAh/g to its half-cell first, first discharging efficiency 90.8%%.
Comparative example 1
Divinylbenzene 300g, hydrochloric acid 100g and naphthalene 1000g are alternately added in reactor under stirring and are mixed, be warming up to
180 DEG C of polymerisations 8 hours, reaction are down to room temperature discharging after terminating, crushed material is crossed 100 eye mesh screens after crushing, load
Well formula retort, being warming up to 500 DEG C under nitrogen protection carries out pre- charing process 5 hours, is cooled to room temperature, will after crushing
Crushed material crosses 100 eye mesh screens, in 1400 DEG C of charing process 5 hours in pushed bat kiln under nitrogen protection, hard carbon cathode is obtained
Material, discharge capacity is 414.3mAh/g to its half-cell first, first discharging efficiency 80.7%.
Comparative example 2
Divinylbenzene 300g, hydrochloric acid 100g and naphthalene 1000g are added in reactor under stirring and are mixed, be warming up to 180 DEG C
Cross-linking reaction and polymerisation 8 hours is carried out, reaction terminates rear temperature and processes 2 hours in 80 DEG C of washing oil toluene Mixed Solvents,
Heat filtering, filter cake vacuum (- 0.09～-0.1MPa, 150 DEG C) are dried 2 hours, are down to room temperature discharging, by powder after crushing
Minced 100 eye mesh screens, in 1400 DEG C of charing process 5 hours in pushed bat kiln under nitrogen protection, hard carbon cathode material is obtained
Material, discharge capacity is 356.5mAh/g to its half-cell first, first discharging efficiency 85.7%.
Comparative example 3
Divinylbenzene 300g, hydrochloric acid 100g and naphthalene 1000g are added in reactor under stirring and are mixed, be warming up to 180 DEG C
Polymerisation 8 hours, reaction terminate rear temperature and process 2 hours in 80 DEG C of washing oil toluene Mixed Solvents, and heat filtering, filter cake are true
Empty (- 0.09～-0.1MPa, 150 DEG C) is dried 2 hours, is down to room temperature discharging, crushed material is crossed 100 mesh sieves after crushing
Net, loads well formula retort, and being warming up to 500 DEG C under nitrogen protection carries out pre- charing process 5 hours, is down to room temperature, powder
Crushed material is crossed into 100 eye mesh screens after broken, in 700 DEG C of charing process 5 hours in pushed bat kiln under nitrogen protection, is obtained hard
Carbon negative pole material, discharge capacity is 343.9mAh/g to its half-cell first, first discharging efficiency 78.5%.
Half-cell method of testing used by of the invention is：Hard carbon sample, the N- crassitudes containing 6～7% Kynoar
Ketone and 2% conductive black are well mixed, and are applied on Copper Foil, and the pole piece for coating is put into temperature for 110 DEG C of vacuum drying chambers
It is middle vacuum drying 4 hours it is standby.Simulated battery is carried out in being assemblied in the German Braun glove box of applying argon gas, and electrolyte is 1M
LiPF6+EC: DEC: DMC=1: 1: 1 (volume ratio), metal lithium sheet are that electrochemical property test is in the U.S. to electrode
Carry out on ArbinBT2000 type cell testers, charging/discharging voltage scope is 0.005 to 1.0V, and charge-discharge velocity is 0.1C.
Used by of the invention, full battery testing method is：The hard carbon of the embodiment of the present invention or comparative example's example makees negative pole, cobalt acid
Lithium makees positive pole, and 1M LiPF6+EC: DMC: EMC=1: 1: 1 (volume ratio) solution is made electrolyte assembling and helps battery, tests
5000 weeks capability retentions of 1C charge and discharges are more than 80%.
The scanning electron microscope (SEM) photograph of hard carbon cathode material by obtained in the present invention is as shown in Figure 1.Embodiment of the present invention 1-8 and contrast are real
The performance parameter for applying a 1-3 is as shown in table 2.
Table 2
The discharging efficiency of comparative example 1 is low, is 80.7%；The discharge capacity of comparative example 2 is low, is 356.5mAh/g；
The discharge capacity of comparative example 3 and discharging efficiency are all low；The hard carbon cathode material prepared using this patent methods described, is put
Up to more than 450mAh/g, discharging efficiency more than 90%, reduces the loss of irreversible capacity to capacitance first, reduces positive pole
Consumption；Battery has a safety feature；Over-charging is preferable；Pole piece processability is good；Preferably charging and discharging curve, is adapted to big
Current charge-discharge electricity；Good cycle, after circulating 5000 times, capability retention can reach more than 80%.
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 do not carrying on the back
In the case of the spirit or essential attributes of the present invention, the present invention can be realized in other specific forms.Therefore, no matter from
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit is required rather than described above is limited, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only included
One independent technical scheme, this narrating mode of specification are only that for clarity, those skilled in the art should be by
Specification as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, forming those skilled in the art can
With the other embodiment for understanding.
Claims (7)
1. a kind of preparation method of lithium ion cell high-capacity hard carbon cathode material, it is characterised in that it include as
Lower step：1. organic matter and alkenyl arene are carried out into polymerisation, obtains polymer；2. by polymer 50～
100 DEG C carry out solvent extraction and process 2～6 hours；3. vacuum drying treatment, is cooled to room temperature, crushes and screens；
4., under inert gas shielding, in 300～650 DEG C of pre- charing low temperature modifier treatment, room temperature is cooled to, is crushed
Screening；5., under inert gas shielding, process in 900～1900 DEG C of high temperature carbonizations and obtain final product.
2. the preparation method of lithium ion cell high-capacity hard carbon cathode material according to claim 1, which is special
Levy and be, step 1. in, organic matter be naphthalene, anthracene, phenanthrene, epoxy resin or phenolic resin.
3. the preparation method of lithium ion cell high-capacity hard carbon cathode material according to claim 1, which is special
Levy and be, alkenyl arene of the alkenyl arene for carbon atom 8～10.
4. the preparation method of lithium ion cell high-capacity hard carbon cathode material according to claim 1, which is special
Levy and be, polymerization reaction time is 1～15 hour；Polymeric reaction temperature is 50～300 DEG C.
5. the preparation method of lithium ion cell high-capacity hard carbon cathode material according to claim 1, which is special
Levy and be, step 2. in, solvent is the mixture of one or more of washing oil, quinoline, toluene, dimethylbenzene.
6. the preparation method of lithium ion cell high-capacity hard carbon cathode material according to claim 1, which is special
Levy and be, step 3. in vacuum drying treatment adopt vacuum drying chamber, step 4. in pre- charing low temperature it is quenched
Process using well formula retort, step 5. in high temperature carbonization process using pushed bat kiln high temperature carbonization furnace.
7. preparation method as described in claim 1-6 is arbitrary is obtained lithium ion battery negative material.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102479942A (en) * | 2010-11-30 | 2012-05-30 | 上海杉杉科技有限公司 | Hard carbon negative electrode material, its preparation method and application |
| CN104600258A (en) * | 2014-12-26 | 2015-05-06 | 宁夏共享新能源材料有限公司 | Composite negative pole material for lithium ion batteries and preparation method thereof |
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- 2015-09-13 CN CN201510581373.7A patent/CN106532050A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102479942A (en) * | 2010-11-30 | 2012-05-30 | 上海杉杉科技有限公司 | Hard carbon negative electrode material, its preparation method and application |
| CN104600258A (en) * | 2014-12-26 | 2015-05-06 | 宁夏共享新能源材料有限公司 | Composite negative pole material for lithium ion batteries and preparation method thereof |
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