CN110407204A - A kind of Preparation method and use of coke low temperature graphitization - Google Patents
A kind of Preparation method and use of coke low temperature graphitization Download PDFInfo
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- CN110407204A CN110407204A CN201910829969.2A CN201910829969A CN110407204A CN 110407204 A CN110407204 A CN 110407204A CN 201910829969 A CN201910829969 A CN 201910829969A CN 110407204 A CN110407204 A CN 110407204A
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- coke
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
Abstract
A kind of Preparation method and use of coke low temperature graphitization, comprising: mixing --- it obtains monoatomic metal and disperses coke composite material；Ultra low temperature vacuum freeze-drying --- the hetero atoms such as hydrogen-oxygen sulphur are sloughed in catalysis, and obtain inferior stable state metal/carbon composite；1400 DEG C of catalysis inferior stable state carbon materials continue regular graphitization, and high purity battery level graphite material is obtained after pickling impurity removal.It is an object of the invention to significantly reduce traditional coke graphitization temperature, 1400 DEG C are reduced to from 2600 DEG C；And the cathode graphite material of function admirable is provided for lithium ion battery.This method has the characteristics that technological operation is simple, repeatability is high, low in cost.
Description
Technical field
The present invention relates to artificial graphite technical field more particularly to a kind of preparation methods and use of coke low temperature graphitization
On the way.
Background technique
Because it is high with output voltage, the long advantage of service life cycle has been widely used for portable lithium ion battery
Formula mobile device.Its main negative electrode material is the regular graphite of height.Graphite is divided into natural graphite and artificial stone according to source
Ink.Natural graphite impurity content is high, and degree of graphitization is relatively poor, it is difficult to meet performance of lithium ion battery demand.Therefore
Lithium ion battery grade graphite is generally artificial graphite.In numerous artificial graphites, coke is its primary raw material, generally requires and drips
The auxiliary materials such as blueness, which pass through, to be greater than 2600 DEG C of high temperature graphitizations and is made, such as patent CN102381700B, CN104609412A with
CN101648808B.It is huge that high temperature (> 2600 DEG C) graphitization technique consumes electricity, and working condition is dangerous, therefore develops low temperature
Graphitization technique can greatly reduce power consumption and production cost, and can be reduced the risk of production environment.
Summary of the invention
The present invention is to solve the graphited high energy consumption issues of above-mentioned high temperature (> 2600 DEG C), and it is monatomic to provide a kind of metal
Graphited preparation method under catalytic coke lower temperature has specific capacity high, recycles as lithium ion battery negative material
The good advantage of stability.
The technical solution used in the present invention:
A kind of preparation method of coke low temperature graphitization, preparation step are as follows:
(1) 1~50g size is taken to be added in 35~150ml organic solvent in 500 mesh coke below, add 0.5~
Mixture is stirred 12h at 10 DEG C by 3g metal chlorination salt；
(2) said mixture is placed in freeze-dryer, in -40~-50 DEG C of progress vacuum freeze drying 12h；It obtains
The ultrapure nanocarbon/metal composite material of inferior stable state；
(3) above-mentioned composite material is calcined into 2~12h at 1400 DEG C under argon atmosphere, product is clear with 0.5M HCl solution
Metal impurities are removed in washout, and the 10h LITHIUM BATTERY graphite material regular to get height is dried then at 60 DEG C.
In the step (1) coke be added organic solvent be N-Methyl pyrrolidone, dimethyl sulfoxide, carbon tetrachloride and
Any one in tetrahydrofuran.
Coke in the step (1) is any one in pitch coke, calcined coke and needle coke.
Metal chlorination salt in the step (1) is any one in ferric trichloride, Nickel Chloride and cobalt chloride.
The graphite of the coke low temperature graphitization is as lithium ion battery negative material.
The operation principle of the present invention is that:
Under vacuum ultra-low temperature surroundings, metal is monatomic can hydrogen (H) and oxygen (O) in catalytic coke, sulphur (S) and oxygen (O)
With water (H2) and sulfur dioxide (SO O2) gaseous state be precipitated, monatomic catalyst can expose more crystal faces and defective bit, be catalyzed
Active sites are far more than the same component catalyst of other large scales, to leave a large amount of defective bits in coke body construction.Defective bit
It is high to locate specific surface energy, the monatomic further catalysis amorphous carbon of metal carries out reconstruction, but because its temperature is low, can not overcome stone
Black esd resistance, to obtain inferior stable state carbon structure.This inferior stable state carbon structure can further overcome graphitization at 1400 DEG C
Resistance is graphitized under the action of catalyst, obtains the very high LITHIUM BATTERY graphite of regularity.
Beneficial effects of the present invention: the present invention can be such that coke is graphitized at 1400 DEG C, greatly reduce graphitization temperature,
Power consumption can be substantially reduced.The artificial graphite for using this method to prepare has specific capacity height as lithium ion battery negative material,
The characteristics of good cycling stability.In addition, this method have the characteristics that it is easy to operate, repeated high, low in cost.
Detailed description of the invention
Fig. 1 is the XRD diagram of the graphite material prepared in embodiment 1 to 4.
Fig. 2 is the SEM figure of the graphite material prepared in embodiment 1 to 4.
Fig. 3 is the XPS map of the vacuum freeze drying catalytic coke carbonized product prepared in embodiment 1 to 4.
Fig. 4 is the transverse electric stream charging and discharging curve figure of the graphite material for preparing as lithium cell cathode material in embodiment 1.
Fig. 5 is the stable circulation performance figure of the graphite material for preparing as lithium cell cathode material in embodiment 2.
Specific embodiment
Below with reference to embodiment and attached drawing, invention is further described in detail.
Referring to attached drawing, the present invention is a kind of preparation method of coke low temperature graphitization, comprising:
(1) 1~50g size is taken to be added in 35~150ml organic solvent in 500 mesh coke below, add 0.5~
Mixture is stirred 12h at 10 DEG C by 3g metal chlorination salt；
(2) said mixture is placed in freeze-dryer, in -40~-50 DEG C of progress vacuum freeze drying 12h；It obtains
The ultrapure nanocarbon/metal composite material of inferior stable state；
(3) above-mentioned composite material is calcined into 2~12h at 1400 DEG C under argon atmosphere, product is clear with 0.5M HCl solution
Metal impurities are removed in washout, and the 10h LITHIUM BATTERY graphite material regular to get height is dried then at 60 DEG C.
The organic solvent is any one in N-Methyl pyrrolidone, dimethyl sulfoxide, carbon tetrachloride and tetrahydrofuran.
The coke is any one in pitch coke, calcined coke and needle coke.
The metal chlorination salt is any one in ferric trichloride, Nickel Chloride and cobalt chloride.
Embodiment 1 is using this method metal low temp catalytic coke graphitization preparation LITHIUM BATTERY graphite material.
It weighs 1g size to be added in 35ml dimethyl sulfoxide in 500 mesh pitch coke below, adds 0.5g ferric trichloride,
Mixture is stirred into 12h at 10 DEG C.Said mixture is placed in freeze-dryer, in -40~-50 DEG C of progress vacuum refrigerations
Dry 12h；Obtain the ultrapure nanocarbon/metal composite material of inferior stable state.By above-mentioned composite material at 1400 DEG C under argon atmosphere
2h is calcined, product is cleaned with 0.5M HCl solution and removes metal impurities, and the 10h battery regular to get height is dried then at 60 DEG C
Grade graphite material, graphite material are stand-by as lithium cell cathode material.
Embodiment 2 is using this method metal low temp catalytic coke graphitization preparation LITHIUM BATTERY graphite material.
It weighs 10g size to be added in 70ml N-Methyl pyrrolidone in 500 mesh calcined coke below, adds 1g bis-
Mixture is stirred 12h at 10 DEG C by nickel chloride.Said mixture is placed in freeze-dryer, is carried out in -40~-50 DEG C
Vacuum freeze drying 12h；Obtain the ultrapure nanocarbon/metal composite material of inferior stable state.By above-mentioned composite material at 1400 DEG C in argon
2h is calcined under gas atmosphere, product is cleaned with 0.5M HCl solution and removes metal impurities, then at 60 DEG C of drying 10h to get high metric
Whole LITHIUM BATTERY graphite material, graphite material are stand-by as lithium cell cathode material.
Embodiment 3 is using this method metal low temp catalytic coke graphitization preparation LITHIUM BATTERY graphite material.
It weighs 30g size to be added in 100ml carbon tetrachloride in 500 mesh calcined coke below, adds 2g cobalt chloride, it will
Mixture stirs 12h at 10 DEG C.Said mixture is placed in freeze-dryer, it is dry in -40~-50 DEG C of progress vacuum refrigerations
Dry 12h；Obtain the ultrapure nanocarbon/metal composite material of inferior stable state.Above-mentioned composite material is forged under argon atmosphere at 1400 DEG C
2h is burnt, product is cleaned with 0.5M HCl solution and removes metal impurities, and the 10h LITHIUM BATTERY regular to get height is dried then at 60 DEG C
Graphite material.
Embodiment 4 is using this method metal low temp catalytic coke graphitization preparation LITHIUM BATTERY graphite material.
It weighs 50g size to be added in 150ml tetrahydrofuran in 500 mesh calcined coke below, adds 3g ferric trichloride,
Mixture is stirred into 12h at 10 DEG C.Said mixture is placed in freeze-dryer, in -40~-50 DEG C of progress vacuum refrigerations
Dry 12h；Obtain the ultrapure nanocarbon/metal composite material of inferior stable state.By above-mentioned composite material at 1400 DEG C under argon atmosphere
2h is calcined, product is cleaned with 0.5M HCl solution and removes metal impurities, and the 10h battery regular to get height is dried then at 60 DEG C
Grade graphite material.
Referring to attached drawing, Fig. 1 is the XRD diagram of the graphite material prepared in embodiment 1 to 4.Wherein, abscissa is angle；It is vertical
Coordinate is relative intensity.Find out to have obtained the very high graphite material of regularity in figure, it is right respectively for the peak at 26 ° and 54 ° in 2 θ
Answer (002) and (004) diffraction surfaces of graphite.
Fig. 2 is the SEM figure of the graphite material prepared in embodiment 1 to 4.The graphite obtained as seen from the figure is micron-scale
Big sheet.
Fig. 3 is the XPS map of the vacuum freeze drying catalytic coke carbonized product prepared in embodiment 1 to 4, can from figure
To find out, under vacuum ultra-low temperature surroundings, metal it is monatomic can hydrogen (H) and oxygen (O) in catalytic coke, sulphur (S) and oxygen (O) with
Water (H2) and sulfur dioxide (SO O2) gaseous state be precipitated, coke by this portion react after, the content of oxygen is substantially reduced, coke ontology
A large amount of defective bits are left in structure, specific surface energy is high at defective bit, and the percentage composition of carbon significantly rises, it was demonstrated that catalysis
The remarkable result of carbonization.
Fig. 4 is the transverse electric stream charging and discharging curve figure of the graphite material for preparing as lithium cell cathode material, In in embodiment 1
Under 0.1C, first discharge specific capacity 361mAh/g, and coulombic efficiency is up to 93%, comprehensive performance is very excellent.
Fig. 5 is the stable circulation performance figure of the graphite material for preparing as lithium cell cathode material in embodiment 2.In 0.1C
Under current density, after 300 circulations, specific capacity conservation rate is up to 99%.It is good to prove that the graphite material of synthesis has
Structural stability shows good stable circulation performance as lithium ion battery negative material.
The embodiments of the present invention have been described in detail above, but content is only the preferred embodiment of the present invention,
It should not be considered as limiting the scope of the invention.Those skilled in the art can working principle and upper according to the present invention
The specific embodiment that face provides can make various equivalent modifications, equivalent replacement, component increase and decrease and reconfigure, from
And more new embodiments are constituted, any changes and modifications in accordance with the scope of the present application should still belong to
Within patent covering scope of the invention.
Claims (5)
1. a kind of preparation method of coke low temperature graphitization characterized by comprising
(1) it takes 1~50g size to be added in 35~150ml organic solvent in 500 mesh coke below, adds 0.5~3g gold
Belong to chlorate, mixture is stirred into 12h at 10 DEG C；
(2) said mixture is placed in freeze-dryer, in -40~-50 DEG C of progress vacuum freeze drying 12h；It obtains metastable
The ultrapure nanocarbon/metal composite material of stationary state；
(3) above-mentioned composite material is calcined into 2~12h at 1400 DEG C under argon atmosphere, product is cleaned with 0.5M HCl solution and removed
Metal impurities are removed, the 10h LITHIUM BATTERY graphite material regular to get height is dried then at 60 DEG C.
2. a kind of preparation method of coke low temperature graphitization according to claim 1, it is characterised in that: the organic solvent
For any one in N-Methyl pyrrolidone, dimethyl sulfoxide, carbon tetrachloride and tetrahydrofuran.
3. a kind of preparation method of coke low temperature graphitization according to claim 1, it is characterised in that: the coke is drip
Any one in green burnt, calcined coke and needle coke.
4. a kind of preparation method of coke low temperature graphitization according to claim 1, it is characterised in that: the metal chlorination
Salt is any one in ferric trichloride, Nickel Chloride and cobalt chloride.
5. a kind of graphite material of coke low temperature graphitization preparation method preparation, which is characterized in that graphite material is as lithium ion
Cell negative electrode material application.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113443623A (en) * | 2021-07-18 | 2021-09-28 | 陕西则明未来科技有限公司 | Method for reducing graphitization temperature through composite catalysis |
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| US20180183061A1 (en) * | 2016-12-23 | 2018-06-28 | 3M Innovative Properties Company | Graphitic materials and methods of making same |
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2019
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| CN101723356A (en) * | 2009-12-14 | 2010-06-09 | 同济大学 | Method for graphitizing amorphous carbon material at low temperature |
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| CN113443623A (en) * | 2021-07-18 | 2021-09-28 | 陕西则明未来科技有限公司 | Method for reducing graphitization temperature through composite catalysis |
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