CN107324327A - A kind of method and purposes using coal as the direct synthetic graphite material of raw material - Google Patents
A kind of method and purposes using coal as the direct synthetic graphite material of raw material Download PDFInfo
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- CN107324327A CN107324327A CN201710561426.8A CN201710561426A CN107324327A CN 107324327 A CN107324327 A CN 107324327A CN 201710561426 A CN201710561426 A CN 201710561426A CN 107324327 A CN107324327 A CN 107324327A
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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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- 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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- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
It is raw material using coal the invention discloses a kind of method and purposes using coal as the direct synthetic graphite material of raw material, by pore-creating and depth carbonization treatment, carries out high temperature graphitization and obtain：Pore-creating carbonization is carried out to coal first with alkali, the appearance structure that has been obtained again by solvent heat cure simultaneously carries out secondary carbonization, the pore structure of these solidifications is conducive to atom diffusion transport in graphitizing process, last graphitization obtains graphite material, the graphite prepared using the above method is as lithium cell cathode material, it is high with specific capacity, the characteristics of good cycling stability and low cost.
Description
Technical field
The invention belongs to the technical field using coal as the direct synthetic graphite material of raw material, and in particular to one kind is using coal as raw material
The method and purposes of direct synthetic graphite material.
Background technology
The renewable energy technologies such as solar energy, wind energy reach its maturity, and usage amount increases sharply, but its intermittent characteristic causes
They can not continue to power to power network, and the energy storage device such as lithium ion battery can solve this problem.In addition, with electronic vapour
The maturation of driving skills art and popularization, the demand of lithium ion battery are also continuously increased.At present, the negative material of commercial li-ion battery
Mainly graphite.China's graphite ore reserves is few, and grade is low, and generally requiring could be as lithium battery after smelting purifying modified
Negative pole is used.Therefore graphite is prepared using other raw materials to be significant.
Contain substantial amounts of colliery, but its combustion product contamination environment, therefore rationally making for coal in the country of China stratum
With being a big problem.Coal, which is become graphite material, can greatly promote social development.Current patent application publication number has：
CN102101664A, CN201110368169.9 and 201410037552x etc..They are using anthracite as raw material, in graphite
, it is necessary to which adding other raw materials such as pitch, petroleum coke and coal tar carries out batch mixing, isostatic pressed processing and calcine by steps etc. before change,
Petroleum coke, pitch, coal tar etc. is the obtained product that is carbonized by complicated technology depth.Coal is block structure, and specific surface area is small,
Batch mixing, isostatic pressed, the purpose of calcine by steps is them is sufficiently mixed with coal, the other contact of molecular level is reached, in pyrographite
Play a part of the graphitization reaction of catalysis coal during change, the proportioning process and charging technique of these patents are complicated, and graphitization
Temperature height (2500-3200 DEG C) so that technology stability it is difficult to ensure that, production cost is high.
The content of the invention
In order to solve the above problems, the invention provides a kind of method and use using coal as the direct synthetic graphite material of raw material
On the way, it is raw material using coal, by pore-creating and depth carbonization treatment, carries out high temperature graphitization and obtain：Coal is carried out first with alkali
Pore-creating is carbonized, then the appearance structure that has been obtained by solvent heat cure and carries out secondary carbonization, and the pore structure of these solidifications is favourable
The atom diffusion transport in graphitizing process, last graphitization obtains graphite material, and the graphite prepared using this method is as lithium
Cell negative electrode material, it is high with specific capacity, the characteristics of good cycling stability and low cost.
To reach above-mentioned purpose, a kind of preparation that lithium cell negative pole graphite material is directly synthesized using coal as raw material of the present invention
Method comprises the following steps：
Step 1, coal dust is made in coal, according to the mass fraction, it is 2mol/L~7mol/L to take 1 part of coal dust and 2~8 parts of concentration
Alkaline solution mix 10 hours~72 hours；
Step 2, the mixed liquor obtained by step 1 is filtered, the product drying after filtering, under an inert atmosphere 600 DEG C~900
DEG C activation 2 hours~10 hours, product is designated as A；
Step 3, A is placed in the reactor containing solvent, the solvent is used to provide solvent thermal reaction, wherein solvent
Volume accounts for the 30-80% of reactor volume, after stirring, and reactor is placed under the conditions of 120 DEG C~220 DEG C, makes reactor
In substance reaction 3 hours~24 hours, product is designated as B, and the alkali and metal impurities in B are removed with hydrochloric acid, then filters, dries
Dry, product is designated as C；
Step 4, by C under an inert atmosphere, 1800 DEG C~2600 DEG C graphitizations 2 hours~24 hours, produce graphite material.
In the step 1, alkaline solution is one kind or any several in lithium hydroxide, sodium hydroxide or potassium hydroxide solution
The mixture planted.
In the step 3, solvent is one kind or any in water, ethanol, methanol, ethylene glycol, isopropanol or carbon tetrachloride
Several mixtures.
In the step 2 and step 4, inert atmosphere is argon gas or nitrogen atmosphere.
In the step 1, coal is one kind in anthracite, bituminous coal and lignite or any several mixtures.
In the step 1, the mesh number of coal dust is less than 200.
Obtained graphite material is used as lithium cell cathode material in aforementioned manners.
Compared with prior art, the present invention at least has following beneficial technique effect, and the present invention first passes through alkaline solution
Activate pore-creating, coal is become loose structure, while activation and hydro-thermal solid hole, make coal surface composition be changed into class coal tar etc. into
Point, coal graphitization is then catalyzed at a lower temperature.Therefore, this method can greatly simplify technique, without adding petroleum coke, pitch
With the component such as coal tar so that (1800 DEG C~2600 DEG C) realize the graphitization of coal at a lower temperature, with it is simple to operate, can
The characteristics of repeatability is high, with low cost, the degree of graphitization of graphite material prepared using this method is high, is used as lithium ion battery anode material
Expect that specific capacity is high, and good cycling stability.
Brief description of the drawings
Fig. 1 is the X-ray diffractogram of the graphite material prepared in embodiment 1 and 5；
Fig. 2 is the Raman figure of the graphite material prepared in embodiment 1 and 5；
Fig. 3 is the scanning electron microscope (SEM) photograph of the graphite material prepared in embodiment 1 and 5；
Fig. 4 be in embodiment 1 graphite material for preparing as lithium cell cathode material charging and discharging capacity figure；
Fig. 5 be in embodiment 1 graphite material for preparing as lithium cell cathode material cyclic voltammogram；
Fig. 6 be in embodiment 2 graphite material for preparing as charging and discharging curve figure during lithium ion battery negative material；
Fig. 7 be in embodiment 3 graphite material for preparing as charging and discharging curve figure during lithium ion battery negative material.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
It is a kind of using coal as the method for the direct synthetic graphite material of raw material, comprise the following steps：
Step 1, coal dust is made in coal, according to the mass fraction, it is 2mol/L~7mol/L's to take 1 part of coal and 2~8 parts of concentration
Alkaline solution is mixed 10 hours~72 hours；
Step 2, the mixed liquor obtained by step 1 is filtered, the product after filtering is dried, 600 DEG C under an inert atmosphere~
900 DEG C activate 2 hours~10 hours, and product is designated as A；
Step 3, A is placed in the reactor containing solvent, solvent is used for the volume for providing solvent thermal reaction, wherein solvent
The 30-80% of reactor volume is accounted for, after stirring, reactor is placed under the conditions of 120 DEG C~220 DEG C, made in reactor
Substance reaction 3 hours~24 hours, product is designated as B, and the alkali and metal impurities in B are removed with hydrochloric acid, then filters, dries, production
Thing is designated as C；
Step 4, by C under an inert atmosphere, 1800 DEG C~2600 DEG C graphitizations 2 hours~24 hours, produce graphite material.
Wherein：In step 1, the mesh number of coal dust is less than 200, and alkaline solution is lithium hydroxide, sodium hydroxide or potassium hydroxide
One kind or any several mixture in solution；Coal is one kind in anthracite, bituminous coal and lignite or any several mixtures.
In step 3, solvent is one kind or any several in water, ethanol, methanol, ethylene glycol, isopropanol or carbon tetrachloride
Mixture.
In step 2 and step 4, inert atmosphere is argon gas or nitrogen atmosphere.
Obtained graphite material is used as lithium cell cathode material in aforementioned manners.
The present invention operation principle be：Alkali activated coal is used first, pore-creating processing is carried out to coal, then to containing loose structure
Coal derived carbon carry out the solvent heat carbonization treatment of deeper degree, consolidate existing pore structure and skeleton structure, then pass through high temperature
Graphitization processing, obtains coal and derives graphite material.
Embodiment 1
It is a kind of using coal as the method for the direct synthetic graphite material of raw material, comprise the following steps：
Step 1, anthracite is crushed, refine to below 200 mesh, according to the mass fraction, take 1 part of coal and the 2 parts of concentration to be
3mol/L lithium hydroxide solution is mixed 20 hours；
Step 2, the mixed liquor obtained by step 1 is filtered, the product after filtering is dried under the conditions of 80 DEG C, in argon gas atmosphere
Lower 700 DEG C activate 5 hours, and product is designated as A；
Step 3, A is placed in the reactor containing water, the volume of water accounts for the 75% of reactor volume, after stirring,
Reactor is placed in 160 DEG C of environment, makes the substance reaction 16 hours in reactor, product is designated as B, is removed with hydrochloric acid in B
Alkali and metal impurities, then filter, dry, product is designated as C；
Step 4, by C in a nitrogen atmosphere, 2600 DEG C of graphitizations 2 hours, produce graphite material.
Embodiment 2
It is a kind of using coal as the method for the direct synthetic graphite material of raw material, comprise the following steps：
Step 1, by bituminous coal milling, according to the mass fraction, the sodium hydroxide solution that 1 part of coal and 4 parts of concentration are 4mol/L is taken
Mixing 72 hours；
Step 2, the mixed liquor obtained by step 1 is filtered, the product drying after filtering, in a nitrogen atmosphere 800 DEG C of activation 2
Hour, product is designated as A；
Step 3, A is placed in the reactor containing ethanol, wherein the volume ratio of ethanol and reactor is 30%, is stirred
Afterwards, reactor is placed under 220 DEG C of environment, makes the substance reaction 3 hours in reactor, product is designated as B, removed with hydrochloric acid in B
Alkali and metal impurities, then filter, dry, product is designated as C；
Step 4, by C in a nitrogen atmosphere, 2800 DEG C of graphitizations 5 hours, produce graphite material.
Embodiment 3
It is a kind of using coal as the method for the direct synthetic graphite material of raw material, comprise the following steps：
Step 1, by brown coal crushing, it refine to below 200 mesh, according to the mass fraction, it is 7mol/ to take 1 part of coal and 8 parts of concentration
L sodium hydroxide solution is mixed 40 hours；
Step 2, the mixed liquor obtained by step 1 is filtered, the product drying after filtering, under an argon atmosphere 700 DEG C of activation 6
Hour, product is designated as A；
Step 3, A is placed in the reactor containing methanol, wherein the volume ratio of methanol and reactor is 65%, and stirring is equal
After even, reactor is placed under 200 DEG C of environment, makes the substance reaction 14 hours in reactor, product is designated as B, B is removed with hydrochloric acid
In alkali and metal impurities, then filter, dry, product is designated as C；
Step 4, by C under an argon atmosphere, 2200 DEG C of graphitizations 10 hours, produce graphite material.
Embodiment 4
It is a kind of using coal as the method for the direct synthetic graphite material of raw material, comprise the following steps：
Step 1, coal is crushed, refine to below 200 mesh, according to the mass fraction, it is 5mol/L to take 1 part of coal and 5 parts of concentration
Potassium hydroxide solution mix 10 hours；
Step 2, the mixed liquor obtained by step 1 is filtered, the product drying after filtering, in a nitrogen atmosphere 600 DEG C of activation
10 hours, product was designated as A；
Step 3, A is placed in the reactor containing ethylene glycol or isopropanol, wherein ethylene glycol or isopropanol and reactor
Volume ratio is 55%, after stirring, and reactor is placed in 120 DEG C of environment, makes the substance reaction 24 hours in reactor, production
Thing is designated as B, and the alkali and metal impurities in B are removed with hydrochloric acid, then filters, dries, product is designated as C；
Step 4, by C under an argon atmosphere, 1800 DEG C of graphitizations 24 hours, produce graphite material.
Embodiment 5
It is a kind of using coal as the method for the direct synthetic graphite material of raw material, comprise the following steps：
Step 1, coal is crushed, refine to below 200 mesh, according to the mass fraction, it is 2mol/L to take 1 part of coal and 7 parts of concentration
Potassium hydroxide solution mix 30 hours；
Step 2, the mixed liquor obtained by step 1 is filtered, the product drying after filtering, in a nitrogen atmosphere 900 DEG C of activation 3
Hour, product is designated as A；
Step 3, A is placed in the reactor containing carbon tetrachloride, the volume ratio of wherein carbon tetrachloride and reactor is
80%, after stirring, reactor is placed under the conditions of 150 DEG C, makes the substance reaction 20 hours in reactor, product is designated as B,
The alkali and metal impurities in B are removed with hydrochloric acid, then filters, dry, product is designated as C；
Step 4, by C under an argon atmosphere, 2400 DEG C of graphitizations 14 hours, produce graphite material.
Fig. 1 is the XRD (X-ray diffractogram) of the graphite material prepared in embodiment 1 and 5, embodiment 5 and embodiment 1
The somewhat small difference only in the intensity at peak, wherein, abscissa is angle；Ordinate is relative intensity.It can be seen that and obtain in figure
Graphite material, be in 2 θ be graphite at 26.8 ° and 54.8 ° diffraction maximum, it will be seen from figure 1 that the stone prepared using this method
Ink material degree of graphitization is high, and structural regularity is good.
Fig. 2 is the Raman figures (Raman figure) of graphite material prepared by embodiment 1 and 5, and embodiment 5 and embodiment 1 are only at peak
Intensity on somewhat small difference, be D the and G peaks of graphite material respectively at 1351 and 1585 wave numbers in figure, can be with from Fig. 2
Find out, G peak intensities are very high, the graphite material structurally ordered degree prepared using this method is high.
Fig. 3 is the SEM figures (scanning electron microscope (SEM) photograph) of graphite material prepared by embodiment 1 and 5, the stone that embodiment 1 to 5 is prepared
The SEM figures of ink material are identical, and thus figure be can be seen that, graphite platelet structure has been obtained using this method.
Fig. 4 be in embodiment 1 graphite material for preparing as charging and discharging curve figure during lithium ion battery negative material.From
It is 367mAh/g that graphitic carbon material first discharge specific capacity is can be seen that in figure, and coulombic efficiency is up to 86%；Second of electric discharge specific volume
Measure as 349mAh/g.Its charging and discharging capacity and coulombic efficiency is higher.
Fig. 5 be in embodiment 1 graphite material for preparing as cyclic voltammetry curve during lithium ion battery negative material.Figure
In redox peaks (0.247/0.245V) illustrate Lithium-ion embeding deviate from graphite interlayer mechanism.
Fig. 6 be in embodiment 2 graphite material for preparing as charging and discharging curve figure during lithium ion battery negative material.From
It is 353mAh/g that graphitic carbon material first discharge specific capacity is can be seen that in figure, and coulombic efficiency is up to 84%；Second of electric discharge specific volume
Measure as 307mAh/g.Its charging and discharging capacity and coulombic efficiency is higher.
Fig. 7 be in embodiment 3 graphite material for preparing as charging and discharging curve figure during lithium ion battery negative material.From
It is 336mAh/g that graphitic carbon material first discharge specific capacity is can be seen that in figure, and coulombic efficiency is up to 82%；Second of electric discharge specific volume
Measure as 288mAh/g.Its charging and discharging capacity and coulombic efficiency is higher.
The present invention does not limit to above-mentioned cited embodiment, and those skilled in the art can be according to the present invention
Operation principle and embodiment given above, can make it is various it is equivalent change, equivalent replacement, part increase and decrease and
Reconfigure, so as to constitute more new embodiments.
Claims (7)
1. a kind of method using coal as the direct synthetic graphite material of raw material, it is characterised in that comprise the following steps：
Step 1, coal dust is made in coal, according to the mass fraction, takes the alkali that 1 part of coal dust and 2~8 parts of concentration are 2mol/L~7mol/L
Property solution mix 10 hours~72 hours；
Step 2, the mixed liquor obtained by step 1 is filtered, the product drying after filtering, 600 DEG C under an inert atmosphere~900 DEG C work
Change 2 hours~10 hours, product is designated as A；
Step 3, A is placed in the reactor containing solvent, the solvent is used for the volume for providing solvent thermal reaction, wherein solvent
The 30-80% of reactor volume is accounted for, after stirring, reactor is placed under the conditions of 120 DEG C~220 DEG C, made in reactor
Substance reaction 3 hours~24 hours, product is designated as B, and the alkali and metal impurities in B are removed with hydrochloric acid, then filters, dries, production
Thing is designated as C；
Step 4, by C under an inert atmosphere, 1800 DEG C~2600 DEG C graphitizations 2 hours~24 hours, produce graphite material.
2. a kind of method using coal as the direct synthetic graphite material of raw material according to claim 1, it is characterised in that step
In 1, alkaline solution is one kind in lithium hydroxide, sodium hydroxide or potassium hydroxide solution or any several mixture.
3. a kind of method using coal as the direct synthetic graphite material of raw material according to claim 1, it is characterised in that step
In 3, solvent is one kind in water, ethanol, methanol, ethylene glycol, isopropanol or carbon tetrachloride or any several mixtures.
4. a kind of method using coal as the direct synthetic graphite material of raw material according to claim 1, it is characterised in that step
2 and step 4 in, inert atmosphere be argon gas or nitrogen atmosphere.
5. a kind of method using coal as the direct synthetic graphite material of raw material according to claim 1, it is characterised in that step
In 1, coal is one kind in anthracite, bituminous coal and lignite or any several mixtures.
6. a kind of method using coal as the direct synthetic graphite material of raw material according to claim 1, it is characterised in that step
In 1, the mesh number of coal dust is less than 200.
7. the method that cathode of lithium battery graphite material is directly synthesized using coal as raw material in claim 1 to 6 described in any one
Prepared graphite material as lithium cell cathode material purposes.
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| CN108101043A (en) * | 2017-12-21 | 2018-06-01 | 陕西科技大学 | A kind of coal derives the Preparation method and use of artificial graphite material |
| CN111029577A (en) * | 2019-11-12 | 2020-04-17 | 山西沁新能源集团股份有限公司 | Method for blending coal with precursor of crystalline carbon coke powder |
| CN112661149A (en) * | 2020-12-24 | 2021-04-16 | 四川金汇能新材料股份有限公司 | Preparation method of graphite negative electrode material, negative electrode material and lithium ion battery |
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| CN112661149A (en) * | 2020-12-24 | 2021-04-16 | 四川金汇能新材料股份有限公司 | Preparation method of graphite negative electrode material, negative electrode material and lithium ion battery |
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|---|---|
| CN107324327B (en) | 2019-05-24 |
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