CN113594450B - Preparation method of coal-based artificial graphite cathode material for lithium ion battery - Google Patents
Preparation method of coal-based artificial graphite cathode material for lithium ion battery Download PDFInfo
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- CN113594450B CN113594450B CN202110802667.3A CN202110802667A CN113594450B CN 113594450 B CN113594450 B CN 113594450B CN 202110802667 A CN202110802667 A CN 202110802667A CN 113594450 B CN113594450 B CN 113594450B
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- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention provides a preparation method of a coal-based artificial graphite cathode material for a lithium ion battery, which comprises the following steps: step 1: drying, crushing and grading the fine coke powder raw material in sequence; and 2, step: purifying the fine coke powder obtained by the treatment in the step 1 by using hydrofluoric acid; and step 3: carrying out rolling, grinding and shaping treatment on the purified fine coke powder; and 4, step 4: carrying out graphitization treatment on the shaped fine coke powder; and 5: and (5) sequentially carrying out demagnetization, screening and mixing treatment on the material obtained by graphitization in the step (4) to obtain the coal-based artificial graphite cathode material. According to the invention, the hydrofluoric acid purification and graphitization procedures are used for removing the key impurities such as Si, al, ca, mg, fe and the like in the artificial graphite raw material in batches, so that the problem of deep removal of the impurities is solved, and the high-purity artificial graphite is obtained; the prepared cathode material also has excellent electrochemical performance, and simultaneously provides a new production process for the artificial graphite cathode material.
Description
Technical Field
The invention relates to the field of preparation of lithium ion battery materials, in particular to a preparation method of a coal-based artificial graphite cathode material for a lithium ion battery.
Background
Lithium ion secondary batteries (LIBs), which are energy storage devices, are important to research in the field of energy storage because of their advantages, such as high energy density, long cycle life, stable charge and discharge platform, wide operating temperature range, and environmental friendliness.
Since sony corporation adopts a carbon material as a negative electrode material of a commercial lithium ion battery for the first time, the carbon material becomes a mainstream raw material of the negative electrode material of the lithium ion battery. Currently, commercial negative electrode materials mainly include graphite-based carbon materials, amorphous carbon materials, and graphitizable carbon materials. However, natural graphite has the defects of poor low compatibility with electrolyte, poor rate capability, poor stability and poor cycle performance. Meanwhile, the hard carbon irreversible capacity of the amorphous carbon material is too large, which is not beneficial to improving the performance of the lithium ion battery; the soft carbon of the amorphous carbon material has high irreversible capacity during first charge and discharge and low output voltage, and is not generally directly used as a negative electrode material. The soft carbon (including needle coke, coke and intermediate phase carbon microsphere) is mainly used for preparing artificial graphite with better comprehensive performance, wherein the needle coke, the coke and the intermediate phase carbon microsphere can be prepared from coal with abundant reserves and lower price.
Disclosure of Invention
The invention aims to provide a preparation method of a coal-based artificial graphite negative electrode material for a lithium ion battery.
In order to realize the purpose, the invention is realized by the following technical scheme:
the coal-based artificial graphite cathode material for the lithium ion battery is characterized in that the specific surface of the cathode material is less than or equal to 2.5m 2 G, tap density is more than or equal to 1.1g/cm 3 The true density is 2.1-2.2g/cm 3 D10 is 5-7 μm, D50 is 14-16 μm, D90 is 25-30 μm, and D100 is not more than 50 μm.
A preparation method of a coal-based artificial graphite cathode material for a lithium ion battery comprises the following steps:
step 1: drying, crushing and grading the fine coke powder raw material in sequence;
step 2: purifying the fine coke powder obtained by the treatment in the step 1 by using hydrofluoric acid;
and step 3: carrying out rolling, grinding and shaping treatment on the purified fine coke powder;
and 4, step 4: carrying out graphitization treatment on the shaped fine coke powder;
and 5: and (5) sequentially carrying out demagnetization, screening and mixing treatment on the material obtained by graphitization in the step (4) to obtain the graphite cathode material.
Further, in the step 1, the total water content of the fine coke powder is less than or equal to 25 percent, the dry-based ash content is 5 to 15 percent, the dry-based ash-free volatile matter content is less than or equal to 2 percent, the fixed carbon content is more than or equal to 86 percent, and the total sulfur content is less than or equal to 0.7 percent; the granularity of the fine coke powder is less than or equal to 0.5mm.
Further, after the coal coke powder is dried in the step 1, the total water content is less than or equal to 1 percent; after the coal coke powder is crushed, the average grain diameter D50 is 18-22 μm.
Further, the concentration of hydrofluoric acid in the step 2 is 3-19wt%.
Further, the specific process of purifying hydrofluoric acid in the step 2 is as follows: placing the fine coke powder obtained by the treatment in the step 1 into a reaction kettle, adding hydrofluoric acid, keeping the solid-liquid ratio at 1; rinsing the obtained acidic filter cake with deionized water at 40-80 ℃, centrifuging again, and repeating rinsing-centrifuging for 6-9 times until a neutral filter cake is generated; and drying the neutral filter cake obtained by centrifugation.
Furthermore, the total water content of the refined coke powder purified by hydrofluoric acid is less than or equal to 21 percent, and the dry basis ash content is less than or equal to 3 percent.
Further, the particle size distribution of the fine coke powder shaped in the step 3 is as follows: d10 is 5-7 μm, D50 is 14-16 μm, D90 is 25-30 μm, and D100 is not more than 45 μm.
Further, the graphitization in the step 4 needs to go through three stages, wherein the first stage is to heat from room temperature to 1100-1300 ℃ at a heating rate of 2-5 ℃/min, the second stage is to heat to 1800-2000 ℃ at a heating rate of 0.5-3 ℃/min, and the third stage is to heat to 2800-3000 ℃ at a heating rate of 1-4 ℃/min.
Further, the granularity of the material sieved in the step 5 is D100 which is less than or equal to 50 mu m; mixing materialThe granularity D10 of the rear material is 5-7 mu m, the D50 is 14-16 mu m, the D90 is 25-30 mu m, the D100 is less than or equal to 50 mu m, the fixed carbon content is more than or equal to 99.95 percent, and the specific surface is less than or equal to 2.5m 2 G, tap density is more than or equal to 1.1g/cm 3 The true density is 2.1-2.2g/cm 3 。
Compared with the prior art, the invention has the following beneficial effects:
(1) The raw materials of the artificial graphite are divided into three major types, namely coal series, petroleum series and coal and petroleum series mixed series, wherein coal series needle coke, petroleum series needle coke and petroleum coke are widely applied, but the prices of the coal series needle coke, petroleum series needle coke and petroleum coke are generally high. The coke powder generated by crushing coke in the industries of metallurgy, chemical engineering and the like is used as a raw material for producing the negative material of the lithium ion battery, so that the resources can be saved, the cost can be reduced, and the pollution can be reduced.
(2) At present, because the impurities of common raw materials for producing the lithium ion battery negative electrode material, such as needle coke, petroleum coke and the like, are less, the negative electrode material production enterprises rarely use raw material purification processes, and also are difficult to find a lot of published papers about coal-based coke powder purification. This patent provides a simple artificial graphite production flow, has demonstrated that material property possibility has been improved greatly through the purification to the raw materials.
Drawings
FIG. 1 is a process flow diagram of example 1 of the present invention;
fig. 2 is (a) 500 times and (b) 2000 times Scanning Electron Microscope (SEM) images of the anode material of example 1 of the present invention;
fig. 3 is a charge-discharge curve of a button cell of the negative electrode material of example 1 of the present invention;
fig. 4 is a CV curve of a button cell of the negative electrode material of example 1 of the present invention;
fig. 5 is an ac impedance curve for a button cell of the negative electrode material of example 1 of the present invention;
fig. 6 shows charge and discharge curves of (a) 1C and (b) 3C of the cylindrical battery of the negative electrode material of example 1 of the present invention.
Detailed Description
The following examples are given in the detailed description and the specific operation on the premise of the technical solutions of the present invention, but do not limit the protection scope of the patent of the present invention, and all technical solutions obtained by using equivalent alternatives or equivalent variations should fall within the protection scope of the present invention.
Example 1
As shown in fig. 1, a preparation method of a coal-based artificial graphite anode material for a lithium ion battery comprises the following steps:
step 1: fine coke powder with the water content of 20 percent, the ash content of 12.02 percent, the fixed carbon content of 86.38 percent and the granularity of less than or equal to 0.5mm is selected as a raw material, and the fine coke powder is dried to have the water content of less than or equal to 0.2 percent; then sent to a Raymond mill for crushing, and the D50 after crushing is 18.25 mu m; then, classifying by a classifier, and collecting by a cyclone collector to obtain qualified materials;
step 2: placing the qualified material obtained in the step (1) into a reaction kettle, adding hydrofluoric acid with the concentration of 19wt%, keeping the solid-liquid ratio at 1:3, and carrying out solid-liquid separation after fully reacting for 24 h; rinsing the obtained acidic filter cake in a rinsing tank by using deionized water at 65 ℃, centrifuging again, and repeating rinsing and centrifuging operations for 8 times until a neutral filter cake is generated; drying the neutral filter cake obtained by centrifugation, wherein the total moisture of the dried material is 0.1%;
and 3, step 3: carrying out rolling, grinding and shaping treatment on the purified material, wherein the particle size distribution of the shaped material is as follows: d10 is 5-7 μm, D50 is 14-16 μm, D90 is 25-30 μm, and D100 is not more than 45 μm;
and 4, step 4: conveying the shaped material into a graphite crucible, then putting the graphite crucible into an Acheson graphitizing furnace, graphitizing the material in three stages under the protection of high-purity nitrogen, wherein in the first stage, the material is heated from room temperature to 1100-1300 ℃ at the heating rate of 2-5 ℃/min, in the second stage, the material is heated to 1800-2000 ℃ at the heating rate of 0.5-3 ℃/min, and in the third stage, the material is heated to 2800-3000 ℃ at the heating rate of 1-4 ℃/min.
And 5: and (3) demagnetizing, screening and mixing the graphitized material in sequence to obtain the coal-based artificial graphite cathode material, wherein the physical and chemical properties of the material are detailed in table 1.
Fig. 2 is an SEM image of the coal-based artificial graphite negative electrode material, and it can be seen from fig. 2 that the coal-based artificial graphite negative electrode material has a substantially uniform morphology and a relatively obvious layered structure.
The prepared coal-based artificial graphite negative electrode material is uniformly mixed with a binder and a conductive agent, coated on a metal current collector, dried and pressed into a button cell. Fig. 3 is a charge-discharge curve of the button cell, and the test result shows that the specific capacity of the button cell prepared from the negative electrode material is 332.9mAh/g, the first effect is 92.5%, and the details are shown in table 1. Fig. 4 is a CV curve for a button cell battery showing the lithium storage mechanism of the material with artificial graphite. Fig. 5 is an ac impedance profile of a button cell showing the material has a lower impedance, indicating efficient transfer of electrons and charge between the electrolyte and the electrodes.
Table 1 example 1 test data, apparatus and method for negative electrode materials
The cylindrical battery prepared by taking the prepared coal-based artificial graphite cathode material as a cathode and lithium iron phosphate as an anode material has 1C and 3C charge-discharge curves as shown in figure 6, and has a capacity retention ratio of 91.96% after 2000 cycles of 1C charge-discharge and 87.01% after 2000 cycles of 3C charge-discharge.
Example 2
A preparation method of a coal-based artificial graphite cathode material for a lithium ion battery comprises the following steps:
step 1: selecting fine coke powder with the water content of 25 percent, the ash content of 5 percent and the fixed carbon content of 90 percent as a raw material, and drying the fine coke powder with the particle size of less than or equal to 0.5mm to obtain fine coke powder with the water content of less than or equal to 0.2 percent; then sent to a Raymond mill for crushing, and the D50 after crushing is 18 mu m; then, classifying by a classifier, and collecting by a cyclone collector to obtain qualified materials;
and 2, step: placing the qualified material obtained in the step 1 into a reaction kettle, adding hydrofluoric acid with the concentration of 10wt%, keeping the solid-liquid ratio at 1; rinsing the obtained acidic filter cake in a rinsing tank by using deionized water at the temperature of 80 ℃, centrifuging again, and repeating rinsing and centrifuging operations for 8 times until a neutral filter cake is generated; drying the neutral filter cake obtained by centrifugation, wherein the total moisture of the dried material is 0.1%;
and 3, step 3: and (3) carrying out rolling, grinding and shaping treatment on the purified material, wherein the particle size distribution of the shaped material is as follows: d10 is 5-7 μm, D50 is 14-16 μm, D90 is 25-30 μm, and D100 is not more than 45 μm;
and 4, step 4: conveying the shaped material into a graphite crucible, then putting the graphite crucible into an Acheson graphitizing furnace, and graphitizing the material in three stages under the protection of high-purity nitrogen, wherein in the first stage, the material is heated from room temperature to 1100-1300 ℃ at the heating rate of 2-5 ℃/min, in the second stage, the material is heated to 1800-2000 ℃ at the heating rate of 0.5-3 ℃/min, and in the third stage, the material is heated to 2800-3000 ℃ at the heating rate of 1-4 ℃/min;
and 5: and (4) demagnetizing, screening and mixing the graphitized material in sequence to obtain the negative electrode material.
Example 3
A preparation method of a coal-based artificial graphite cathode material for a lithium ion battery comprises the following steps:
step 1: selecting fine coke powder with 20% of water, 15% of ash and 86% of fixed carbon in metallurgical coke and with the granularity of less than or equal to 0.5mm as a raw material, and drying the fine coke powder to obtain fine coke powder with the moisture of less than or equal to 0.2%; then sending to a Raymond mill for crushing, wherein D50 is 22 mu m after crushing; then, classifying by a classifier, and collecting by a cyclone collector to obtain qualified materials;
and 2, step: placing the qualified material obtained in the step (1) into a reaction kettle, adding hydrofluoric acid with the concentration of 3wt%, keeping the solid-liquid ratio at 1:3, and carrying out solid-liquid separation after fully reacting for 24 h; rinsing the obtained acidic filter cake in a rinsing tank by using deionized water at 40 ℃, centrifuging again, and repeating rinsing and centrifuging operations for 8 times until a neutral filter cake is generated; drying the neutral filter cake obtained by centrifugation, wherein the total moisture of the dried material is 0.1%;
and step 3: and (3) carrying out rolling, grinding and shaping treatment on the purified material, wherein the particle size distribution of the shaped material is as follows: d10 is 5-7 μm, D50 is 14-16 μm, D90 is 25-30 μm, and D100 is not more than 45 μm;
and 4, step 4: conveying the shaped material into a graphite crucible, then putting the graphite crucible into an Acheson graphitizing furnace, and graphitizing the material in three stages under the protection of high-purity nitrogen, wherein in the first stage, the material is heated to 1100-1300 ℃ from room temperature at the heating rate of 2-5 ℃/min, in the second stage, the material is heated to 1800-2000 ℃ at the heating rate of 0.5-3 ℃/min, and in the third stage, the material is heated to 2800-3000 ℃ at the heating rate of 1-4 ℃/min;
and 5: and (4) demagnetizing, screening and mixing the graphitized material in sequence to obtain the negative electrode material.
Example 4
A preparation method of a coal-based artificial graphite cathode material for a lithium ion battery comprises the following steps:
step 1: selecting fine coke powder with the water content of 10 percent, the ash content of 10 percent, the fixed carbon content of 88 percent and the granularity of less than or equal to 0.5mm as a raw material, and drying the fine coke powder to ensure that the water content is less than or equal to 0.2 percent; then sending to a Raymond mill for crushing, wherein D50 is 20 mu m after crushing; then, classifying by a classifier, and collecting by a cyclone collector to obtain qualified materials;
and 2, step: placing the qualified material obtained in the step 1 into a reaction kettle, adding hydrofluoric acid with the concentration of 15wt%, keeping the solid-liquid ratio at 1; rinsing the obtained acidic filter cake in a rinsing tank by using deionized water at 60 ℃, centrifuging again, and repeating rinsing and centrifuging operations for 8 times until a neutral filter cake is generated; drying the neutral filter cake obtained by centrifugation, wherein the total water content of the dried material is 0.1%;
and step 3: carrying out rolling, grinding and shaping treatment on the purified material, wherein the particle size distribution of the shaped material is as follows: d10 is 5-7 μm, D50 is 14-16 μm, D90 is 25-30 μm, and D100 is not more than 45 μm;
and 4, step 4: conveying the shaped material into a graphite crucible, then putting the graphite crucible into an Acheson graphitizing furnace, and graphitizing the material in three stages under the protection of high-purity nitrogen, wherein in the first stage, the material is heated from room temperature to 1100-1300 ℃ at the heating rate of 2-5 ℃/min, in the second stage, the material is heated to 1800-2000 ℃ at the heating rate of 0.5-3 ℃/min, and in the third stage, the material is heated to 2800-3000 ℃ at the heating rate of 1-4 ℃/min;
and 5: and (4) demagnetizing, screening and mixing the graphitized material in sequence to obtain the negative electrode material.
Claims (8)
1. A preparation method of a coal-based artificial graphite cathode material for a lithium ion battery is characterized by comprising the following steps:
step 1: drying, crushing and grading the fine coke powder raw material in sequence;
and 2, step: purifying the fine coke powder obtained by the treatment in the step 1 by using hydrofluoric acid;
and step 3: carrying out rolling, grinding and shaping treatment on the purified fine coke powder;
and 4, step 4: graphitizing the shaped fine coke powder;
and 5: carrying out demagnetization, screening and material mixing treatment on the material obtained by graphitization in the step 4 in sequence to obtain the graphite cathode material;
the graphitization in the step 4 needs to go through three stages, wherein the first stage is to heat from room temperature to 1100-1300 ℃ at the heating rate of 2-5 ℃/min, the second stage is to heat to 1800-2000 ℃ at the heating rate of 0.5-3 ℃/min, and the third stage is to heat to 2800-3000 ℃ at the heating rate of 1-4 ℃/min;
the specific surface of the graphite cathode material is less than or equal to 2.5m 2 The tap density is more than or equal to 1.1g/cm 3 The true density is 2.1-2.2g/cm 3 D10 is 5-7 μm, D50 is 14-16 μm, D90 is 25-30 μm, and D100 is not more than 50 μm.
2. The preparation method of the coal-based artificial graphite negative electrode material for the lithium ion battery as claimed in claim 1, wherein in the step 1, the total water content of the fine coke powder is less than or equal to 25%, the dry-based ash content is 5% -15%, the dry-based ashless volatile matter content is less than or equal to 2%, the fixed carbon content is greater than or equal to 86%, and the total sulfur content is less than or equal to 0.7%; the granularity of the fine coke powder is less than or equal to 0.5mm.
3. The preparation method of the coal-based artificial graphite cathode material for the lithium ion battery as claimed in claim 1, wherein the coal coke powder is dried in the step 1, and the total water content is less than or equal to 1%; after the coal coke powder is crushed, the average grain diameter D50 is 18-22 μm.
4. The preparation method of the coal-based artificial graphite anode material for the lithium ion battery as claimed in claim 1, wherein the concentration of hydrofluoric acid in the step 2 is 3-19wt%.
5. The preparation method of the coal-based artificial graphite anode material for the lithium ion battery as claimed in claim 1, wherein the specific process of purifying the hydrofluoric acid in the step 2 is as follows: placing the fine coke powder obtained by the treatment in the step 1 into a reaction kettle, adding hydrofluoric acid, keeping the solid-liquid ratio at 1-3-1; rinsing the obtained acidic filter cake with deionized water at 40-80 ℃, centrifuging again, and repeating rinsing-centrifuging for 6-9 times until a neutral filter cake is generated; and drying the neutral filter cake obtained by centrifugation.
6. The preparation method of the coal-based artificial graphite cathode material for the lithium ion battery as claimed in claim 1, wherein the total water content of the refined coke powder purified by hydrofluoric acid is less than or equal to 21%, and the dry ash content is less than or equal to 3%.
7. The preparation method of the coal-based artificial graphite negative electrode material for the lithium ion battery as claimed in claim 1, wherein the particle size distribution of the fine coke powder shaped in the step 3 is as follows: d10 is 5-7 μm, D50 is 14-16 μm, D90 is 25-30 μm, and D100 is not more than 45 μm.
8. The preparation method of the coal-based artificial graphite negative electrode material for the lithium ion battery as claimed in claim 1, wherein the particle size of the material sieved in the step 5 is D100 ≤ 50 μm; the granularity D10 of the mixed material is 5-7 mu m, the D50 is 14-16 mu m, the D90 is 25-30 mu m, the D100 is less than or equal to 50 mu m, the fixed carbon content is more than or equal to 99.95 percent, and the specific surface is less than or equal to 2.5m 2 The tap density is more than or equal to 1.1g/cm 3 The true density is 2.1-2.2g/cm 3 。
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| CN109081326A (en) * | 2018-08-23 | 2018-12-25 | 石家庄尚太科技有限公司 | A kind of high power lithium ion cell negative electrode material and preparation method thereof |
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