CN107324327B - It is a kind of using coal as the method and purposes of the direct synthetic graphite material of raw material - Google Patents
It is a kind of using coal as the method and purposes of the direct synthetic graphite material of raw material Download PDFInfo
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- H01M10/00—Secondary cells; Manufacture thereof
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Abstract
The invention discloses a kind of using coal as the method and purposes of the direct synthetic graphite material of raw material, it is raw material using coal, by pore-creating and depth carbonization treatment, it carries out high temperature graphitization to obtain: pore-creating carbonization being carried out to coal first with alkali, pass through the appearance structure that solvent heat cure has obtained again and carries out secondary carbonization, these cured pore structures are conducive to atom diffusion transport in graphitizing process, finally graphitization obtains graphite material, using the graphite of above method preparation as lithium cell cathode material, with specific capacity height, good cycling stability and feature at low cost.
Description
Technical field
The invention belongs to using coal as the technical field of 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 technique
The renewable energy technologies such as solar energy, wind energy reach its maturity, and usage amount increases sharply, but its intermittent characteristic causes
They cannot continue to power to power grid, and the energy storage devices such as lithium ion battery can solve this problem.In addition, with electronic vapour
The maturation and popularization of driving skills art, the demand of lithium ion battery are also continuously increased.Currently, the negative electrode material of commercial li-ion battery
Mainly graphite.China's graphite ore reserves is few, and grade is low, generally requires that lithium battery could be used as after smelting purifying modified
Cathode uses.Therefore graphite is prepared using other raw materials to be of great significance.
Contain a large amount of coal mine, but its combustion product contamination environment in the country, China stratum, therefore coal is rationally made
With being a big problem.Coal, which is become graphite material, can greatly push social development.Current patent application publication number has:
CN102101664A, CN201110368169.9 and 201410037552x etc..They are using anthracite as raw material, in graphite
Before change, needs to be added other raw materials such as pitch, petroleum coke and coal tar and carries out mixing, isostatic pressing and calcine by steps etc.,
Petroleum coke, pitch, coal tar etc. are the products being carbonized by complicated technology depth.Coal is block structure, and specific surface area is small,
Mixing waits static pressure, and the purpose of calcine by steps is to be sufficiently mixed them with coal, reaches the other contact of molecular level, in pyrographite
Play the role of being catalyzed coal graphitization reaction during changing, the proportioning process and charging technique of these patents are complicated, and are graphitized
Temperature height (2500-3200 DEG C) so that technology stability it is difficult to ensure that, high production cost.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of using coal as the method and use of 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 carbonization, then the appearance structure that has obtained by solvent heat cure and secondary carbonization is carried out, these cured pore structures are advantageous
The atom diffusion transport in graphitizing process, finally graphitization obtains graphite material, using the graphite of this method preparation as lithium
Cell negative electrode material has specific capacity height, good cycling stability and feature at low cost.
In order to achieve the above objectives, a kind of preparation directly synthesizing lithium cell negative pole graphite material using coal as raw material of the present invention
Method the following steps are included:
Step 1, coal dust is made in coal, according to the mass fraction, taking 1 part of coal dust and 2~8 parts of concentration is 2mol/L~7mol/L
Alkaline solution mix 10 hours~72 hours；
Step 2, the resulting mixed liquor of step 1 is filtered, filtered product drying, under an inert atmosphere 600 DEG C~900
DEG C activation 2 hours~10 hours, product is denoted as A；
Step 3, A is placed in the reaction kettle containing solvent, the solvent is for providing solvent thermal reaction, wherein solvent
Volume accounts for the 30-80% of reaction kettle volume, after mixing evenly, under the conditions of reaction kettle is placed in 120 DEG C~220 DEG C, makes reaction kettle
In substance reaction 3 hours~24 hours, product is denoted as B, with hydrochloric acid remove B in alkali and metal impurities, then filter, dry
Dry, product is denoted as C；
Step 4, under an inert atmosphere by C, 1800 DEG C~2600 DEG C are graphitized 2 hours~24 hours to get graphite material.
In the step 1, alkaline solution is one of lithium hydroxide, sodium hydroxide or potassium hydroxide solution or any several
The mixture of kind.
In the step 3, solvent is for one of water, ethyl alcohol, methanol, ethylene glycol, isopropanol or carbon tetrachloride or arbitrarily
Several mixtures.
In the step 2 and step 4, inert atmosphere is argon gas or nitrogen atmosphere.
In the step 1, coal is one of anthracite, bituminous coal and lignite or any several mixtures.
In the step 1, the mesh number of coal dust is less than 200.
Graphite material obtained is as lithium cell cathode material in aforementioned manners.
Compared with prior art, the present invention at least has technical effect beneficial below, and the present invention first passes through alkaline solution
Activate pore-creating, coal made to become porous structure, while activation and hydro-thermal solid hole, make coal surface composition become class coal tar etc. at
Point, then catalysis coal is graphitized at a lower temperature.Therefore, this method can greatly simplify technique, without adding petroleum coke, pitch
With the components such as coal tar, thus the graphitization of (1800 DEG C~2600 DEG C) realization coals at a lower temperature, have it is easy to operate, can
Repeated high, feature low in cost, the degree of graphitization of graphite material using this method preparation is high, as lithium ion battery anode material
Expect that specific capacity is high, and good cycling stability.
Detailed description of the invention
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 is the charging and discharging capacity figure of the graphite material for preparing as lithium cell cathode material in embodiment 1；
Fig. 5 is the cyclic voltammogram of the graphite material for preparing as lithium cell cathode material in embodiment 1；
Fig. 6 is the charging and discharging curve figure when graphite material for preparing is as lithium ion battery negative material in embodiment 2；
Fig. 7 is the charging and discharging curve figure when graphite material for preparing is as lithium ion battery negative material in embodiment 3.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A method of using coal as the direct synthetic graphite material of raw material, including the following steps:
Step 1, coal dust is made in coal, according to the mass fraction, taking 1 part of coal and 2~8 parts of concentration is 2mol/L~7mol/L's
Alkaline solution mixes 10 hours~72 hours；
Step 2, the resulting mixed liquor of step 1 is filtered, filtered product is dried, 600 DEG C under an inert atmosphere~
900 DEG C activate 2 hours~10 hours, and product is denoted as A；
Step 3, A is placed in the reaction kettle containing solvent, solvent is used to provide solvent thermal reaction, wherein the volume of solvent
The 30-80% of reaction kettle volume is accounted for, after mixing evenly, under the conditions of reaction kettle is placed in 120 DEG C~220 DEG C, is made in reaction kettle
Substance reaction 3 hours~24 hours, product was denoted as B, removed the alkali and metal impurities in B with hydrochloric acid, then filters, dries, produces
Object is denoted as C；
Step 4, under an inert atmosphere by C, 1800 DEG C~2600 DEG C are graphitized 2 hours~24 hours to get graphite material.
Wherein: in step 1, for the mesh number of coal dust less than 200, alkaline solution is lithium hydroxide, sodium hydroxide or potassium hydroxide
One of solution or any several mixture；Coal is one of anthracite, bituminous coal and lignite or any several mixtures.
In step 3, solvent is one of water, ethyl alcohol, methanol, ethylene glycol, isopropanol or carbon tetrachloride or any several
Mixture.
In step 2 and step 4, inert atmosphere is argon gas or nitrogen atmosphere.
Graphite material obtained is as lithium cell cathode material in aforementioned manners.
The operation principle of the present invention is that: alkali activated coal is used first, pore-creating processing is carried out to coal, then to containing porous structure
Coal derived carbon carry out deeper degree solvent heat carbonization treatment, consolidate existing pore structure and skeleton structure, then pass through high temperature
Graphitization processing obtains the derivative graphite material of coal.
Embodiment 1
A method of using coal as the direct synthetic graphite material of raw material, including the following steps:
Step 1, anthracite is crushed, refine to 200 mesh hereinafter, according to the mass fraction, taking 1 part of coal and 2 parts of concentration being
The lithium hydroxide solution of 3mol/L mixes 20 hours；
Step 2, the resulting mixed liquor of step 1 is filtered, filtered product is dried under the conditions of 80 DEG C, in argon atmosphere
Lower 700 DEG C activate 5 hours, and product is denoted as A；
Step 3, A being placed in the reaction kettle containing water, the volume of water accounts for the 75% of reaction kettle volume, after mixing evenly,
Reaction kettle is placed in 160 DEG C of environment, substance reaction 16 hours in reaction kettle are made, product is denoted as B, is removed in B with hydrochloric acid
Then alkali and metal impurities are filtered, are dried, product is denoted as C；
Step 4, in a nitrogen atmosphere by C, 2 hours are graphitized to get graphite material for 2600 DEG C.
Embodiment 2
A method of using coal as the direct synthetic graphite material of raw material, including the following steps:
Step 1, by bituminous coal milling, according to the mass fraction, take 1 part of coal and 4 parts of concentration for the sodium hydroxide solution of 4mol/L
Mixing 72 hours；
Step 2, the resulting mixed liquor of step 1 is filtered, filtered product drying, 800 DEG C of activation 2 in a nitrogen atmosphere
Hour, product is denoted as A；
Step 3, A is placed in the reaction kettle containing ethyl alcohol, wherein the volume ratio of ethyl alcohol and reaction kettle is 30%, is stirred evenly
Afterwards, reaction kettle is placed under 220 DEG C of environment, makes substance reaction 3 hours in reaction kettle, product is denoted as B, is removed in B with hydrochloric acid
Alkali and metal impurities, then filter, dry, product is denoted as C；
Step 4, in a nitrogen atmosphere by C, 5 hours are graphitized to get graphite material for 2800 DEG C.
Embodiment 3
A method of using coal as the direct synthetic graphite material of raw material, including the following steps:
Step 1, by brown coal crushing, 200 mesh are refine to hereinafter, according to the mass fraction, taking 1 part of coal and 8 parts of concentration is 7mol/
The sodium hydroxide solution of L mixes 40 hours；
Step 2, the resulting mixed liquor of step 1 is filtered, filtered product drying, 700 DEG C of activation 6 under an argon atmosphere
Hour, product is denoted as A；
Step 3, A is placed in the reaction kettle containing methanol, wherein the volume ratio of methanol and reaction kettle is 65%, and stirring is equal
After even, reaction kettle is placed under 200 DEG C of environment, makes substance reaction 14 hours in reaction kettle, product is denoted as B, removes B with hydrochloric acid
In alkali and metal impurities, then filter, dry, product is denoted as C；
Step 4, under an argon atmosphere by C, 10 hours are graphitized to get graphite material for 2200 DEG C.
Embodiment 4
A method of using coal as the direct synthetic graphite material of raw material, including the following steps:
Step 1, coal is crushed, refine to 200 mesh hereinafter, according to the mass fraction, taking 1 part of coal and 5 parts of concentration is 5mol/L
Potassium hydroxide solution mix 10 hours；
Step 2, the resulting mixed liquor of step 1 is filtered, filtered product drying, 600 DEG C of activation in a nitrogen atmosphere
10 hours, product was denoted as A；
Step 3, A is placed in the reaction kettle containing ethylene glycol or isopropanol, wherein ethylene glycol or isopropanol and reaction kettle
Volume ratio is 55%, and after mixing evenly, reaction kettle is placed in 120 DEG C of environment, makes substance reaction 24 hours in reaction kettle, is produced
Object is denoted as B, removes the alkali and metal impurities in B with hydrochloric acid, then filters, dries, product is denoted as C；
Step 4, under an argon atmosphere by C, 24 hours are graphitized to get graphite material for 1800 DEG C.
Embodiment 5
A method of using coal as the direct synthetic graphite material of raw material, including the following steps:
Step 1, coal is crushed, refine to 200 mesh hereinafter, according to the mass fraction, taking 1 part of coal and 7 parts of concentration is 2mol/L
Potassium hydroxide solution mix 30 hours；
Step 2, the resulting mixed liquor of step 1 is filtered, filtered product drying, 900 DEG C of activation 3 in a nitrogen atmosphere
Hour, product is denoted as A；
Step 3, A is placed in the reaction kettle containing carbon tetrachloride, wherein the volume ratio of carbon tetrachloride and reaction kettle is
80%, after mixing evenly, under the conditions of reaction kettle is placed in 150 DEG C, make substance reaction 20 hours in reaction kettle, product is denoted as B,
The alkali and metal impurities in B are removed with hydrochloric acid, then filters, dry, product is denoted as C；
Step 4, under an argon atmosphere by C, 14 hours are graphitized to get graphite material for 2400 DEG C.
Fig. 1 is the XRD diagram (X-ray diffractogram) of the graphite material prepared in embodiment 1 and 5, embodiment 5 and embodiment 1
The only somewhat small difference in the intensity at peak, wherein abscissa is angle；Ordinate is relative intensity.It can be seen that obtain in figure
Graphite material, in the diffraction maximum of 2 θ to be at 26.8 ° and 54.8 ° be graphite, 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 that the Raman of graphite material prepared by embodiment 1 and 5 schemes (Raman figure), and embodiment 5 and embodiment 1 are only at peak
Intensity on somewhat small difference, be the peak D and G of graphite material respectively at 1351 and 1585 wave numbers in figure, can be with from Fig. 2
Find out, G peak intensity is very high, and the graphite material structurally ordered degree using this method preparation is high.
Fig. 3 is that the SEM of graphite material prepared by embodiment 1 and 5 schemes (scanning electron microscope (SEM) photograph), the stone that embodiment 1 to 5 is prepared
The SEM figure of ink material is identical, and thus figure can be seen that, obtain graphite platelet structure using this method.
Fig. 4 is the charging and discharging curve figure when graphite material for preparing is as lithium ion battery negative material in embodiment 1.From
It can be seen that graphitic carbon material first discharge specific capacity is 367mAh/g in figure, coulombic efficiency is up to 86%；Second of electric discharge specific volume
Amount is 349mAh/g.Its charging and discharging capacity and coulombic efficiency is higher.
Fig. 5 is the cyclic voltammetry curve when graphite material for preparing is as lithium ion battery negative material in embodiment 1.Figure
In redox peaks (0.247/0.245V) illustrate lithium ion insertion abjection graphite interlayer mechanism.
Fig. 6 is the charging and discharging curve figure when graphite material for preparing is as lithium ion battery negative material in embodiment 2.From
It can be seen that graphitic carbon material first discharge specific capacity is 353mAh/g in figure, coulombic efficiency is up to 84%；Second of electric discharge specific volume
Amount is 307mAh/g.Its charging and discharging capacity and coulombic efficiency is higher.
Fig. 7 is the charging and discharging curve figure when graphite material for preparing is as lithium ion battery negative material in embodiment 3.From
It can be seen that graphitic carbon material first discharge specific capacity is 336mAh/g in figure, coulombic efficiency is up to 82%；Second of electric discharge specific volume
Amount is 288mAh/g.Its charging and discharging capacity and coulombic efficiency is higher.
The present invention does not limit to above-mentioned cited specific embodiment, and those skilled in the art can be according to the present invention
Working principle and specific embodiment given above, can make various equivalent modifications, equivalent replacement, component increase and decrease and
It reconfigures, to constitute more new embodiments.
Claims (6)
1. a kind of using coal as the method for the direct synthetic graphite material of raw material, characterized in that it comprises the following steps:
Step 1, coal dust is made in coal, according to the mass fraction, takes 1 part of coal dust and 2~8 parts of concentration for the alkali of 2mol/L~7mol/L
Property solution mix 10 hours~72 hours；
Step 2, the resulting mixed liquor of step 1 is filtered, filtered product drying, 600 DEG C under an inert atmosphere~900 DEG C work
Change 2 hours~10 hours, product is denoted as A；
Step 3, A is placed in the reaction kettle containing solvent, the solvent is used to provide solvent thermal reaction, wherein the volume of solvent
The 30-80% of reaction kettle volume is accounted for, after mixing evenly, under the conditions of reaction kettle is placed in 120 DEG C~220 DEG C, is made in reaction kettle
Substance reaction 3 hours~24 hours, product was denoted as B, removed the alkali and metal impurities in B with hydrochloric acid, then filters, dries, produces
Object is denoted as C；
Step 4, under an inert atmosphere by C, 1800 DEG C~2600 DEG C are graphitized 2 hours~24 hours to get graphite material.
2. according to claim 1 a kind of using coal as the method for the direct synthetic graphite material of raw material, which is characterized in that step
In 1, alkaline solution is one of lithium hydroxide, sodium hydroxide or potassium hydroxide solution or any several mixture.
3. according to claim 1 a kind of using coal as the method for the direct synthetic graphite material of raw material, which is characterized in that step
In 3, solvent is one of water, ethyl alcohol, methanol, ethylene glycol, isopropanol or carbon tetrachloride or any several mixtures.
4. according to claim 1 a kind of using coal as the method for the direct synthetic graphite material of raw material, which is characterized in that step
2 and step 4 in, inert atmosphere be argon gas or nitrogen atmosphere.
5. according to claim 1 a kind of using coal as the method for the direct synthetic graphite material of raw material, which is characterized in that step
In 1, coal is one of anthracite, bituminous coal and lignite or any several mixtures.
6. according to claim 1 a kind of using coal as the method for the direct synthetic graphite material of raw material, which is characterized in that step
In 1, the mesh number of coal dust is less than 200.
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| CN108101043B (en) * | 2017-12-21 | 2021-05-18 | 陕西科技大学 | Preparation method and application of coal-derived artificial graphite material |
| CN111029577B (en) * | 2019-11-12 | 2023-09-29 | 山西沁新能源集团股份有限公司 | Method for blending crystalline coke powder precursor coal |
| 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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| US6245460B1 (en) * | 1997-08-28 | 2001-06-12 | Samsung Display Devices Co., Ltd. | Negative electrode active material for lithium-based secondary battery and method of preparing same |
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| JP2015053291A (en) * | 2014-12-01 | 2015-03-19 | 三菱化学株式会社 | Method for manufacturing graphite material for lithium ion secondary battery, negative electrode for lithium ion secondary battery, and lithium ion secondary battery |
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| US5888469A (en) * | 1995-05-31 | 1999-03-30 | West Virginia University | Method of making a carbon foam material and resultant product |
| US6245460B1 (en) * | 1997-08-28 | 2001-06-12 | Samsung Display Devices Co., Ltd. | Negative electrode active material for lithium-based secondary battery and method of preparing same |
| CN101108729A (en) * | 2006-07-20 | 2008-01-23 | 天津市铁诚电池材料有限公司 | Method for manufacturing artificial plumbago negative pole material of lithium ion power cell |
| JP2015053291A (en) * | 2014-12-01 | 2015-03-19 | 三菱化学株式会社 | Method for manufacturing graphite material for lithium ion secondary battery, negative electrode for lithium ion secondary battery, and lithium ion secondary battery |
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