CN114437557A - Preparation method of high-softening-point coated asphalt for lithium ion battery negative electrode material - Google Patents
Preparation method of high-softening-point coated asphalt for lithium ion battery negative electrode material Download PDFInfo
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Abstract
The invention relates to a preparation method of high-softening-point coated asphalt for a lithium ion battery cathode material. The coated asphalt prepared by the process method has good ductility and high coking value, and can be cracked on the surface and in the graphite under the high-temperature inert condition to form a compact amorphous carbon layer, so that cracks and cavities on the surface of the graphite are repaired, the active end faces on the surface of the graphite are reduced, and the electrochemical performance of the graphite cathode is further improved.
Description
Technical Field
The invention relates to the technical field of coal tar pitch deep processing; in particular to a preparation method of high-softening-point coated asphalt for a lithium ion battery cathode material.
Background
The lithium ion battery is used as a new generation of energy storage power supply, has the advantages of high energy density, long cycle life, small self-discharge, wide working temperature range, environmental friendliness and the like, and is widely applied to the mainstream power supply of small energy storage devices such as mobile phones, notebook computers, cameras, toys for children and the like. In recent years, with the continuous improvement of the production technology of the lithium ion battery, the application of the lithium ion battery is gradually expanded to high and new technical fields such as electric vehicles, mobile communication, military equipment, aerospace and the like.
The cathode material is used as a core component of the lithium ion battery and can meet the conditions of high specific capacity, long cycle life, high conductivity, simple preparation process and the like. The graphite carbon material has the advantages of low charge-discharge voltage platform, large lithium ion diffusion coefficient, good conductivity and the like, and is a negative electrode material mainly adopted by the current lithium ion battery. With the rapid development of the new energy automobile industry, the market demand of the lithium ion power battery is greatly increased, and higher requirements are made on physical and chemical indexes of the negative electrode material, such as granularity, specific surface area, tap density, energy density, cycle life, rate capability and the like. The graphite carbon material has poor compatibility with electrolyte, poor stability of crystal structure, easy damage of surface crystal structure in the charging and discharging process, and serious influence on the charging and discharging performance of the battery, so the requirement of high-performance cathode material cannot be met.
The coating modification treatment can effectively improve the surface defects of the graphite carbon material, reduce the specific surface area of the negative electrode material and improve the first charge-discharge efficiency and the cycle performance. The coating material can be cracked at high temperature to form a layer of compact amorphous carbon attached to the surface of graphite to repair cavities and cracks on the surface of the graphite-like carbon material, and the interlayer spacing of the amorphous carbon material is larger than that of the graphite, so that Li in the charge-discharge process can be improved+The diffusion property of (c). Meanwhile, the attached amorphous carbon can also reduce the active end face on the graphite surface, thereby avoiding the decomposition of electrolyte on the active end face on the graphite surface and improving the multiplying power and the cycle performance of the graphite material.
At present, no clear standard exists in the industry about which property of asphalt should be selected for coating the graphite negative electrode, the existing coating material is oil-based or coal-based asphalt with different softening points, the quality characteristics of the asphalt, such as the softening point, the coking value, the content of quinoline insoluble substances, and the like, are different, the problems of poor coating uniformity, difficulty in completely coating the graphite, only coating the asphalt on the surface of the graphite, no penetration into the inner pores of graphite particles, and the like often occur after coating, the expected coating effect is difficult to achieve, and the requirement of a power battery on the negative electrode material cannot be met. Therefore, the preparation of the high-softening-point coating asphalt specially suitable for the coating process has important significance for the future development of the lithium ion battery cathode material.
Disclosure of Invention
The invention aims to provide a preparation method of high-softening-point coated asphalt for a lithium ion battery cathode material. The added modifier can improve the rheological property of the coated asphalt, so that the coated asphalt can penetrate into the pores in the graphite particles. The coated asphalt prepared by the process method has good ductility and high coking value, and can be cracked on the surface and in the graphite under the high-temperature inert condition to form a compact amorphous carbon layer, so that cracks and cavities on the surface of the graphite are repaired, the active end faces on the surface of the graphite are reduced, and the electrochemical performance of the graphite cathode is further improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of high-softening-point coated asphalt for a lithium ion battery negative electrode material comprises the following steps:
1) taking medium-temperature coal pitch as a raw material, adding petroleum pitch into the medium-temperature coal pitch, and uniformly mixing the two kinds of pitch in a reaction kettle with a heating and stirring device to prepare mixed pitch;
2) adding an organic solvent into the mixed asphalt by adopting a solvent extraction method to remove high-viscosity residue precipitate, and performing primary purification treatment; performing secondary purification treatment on the mixed asphalt without the high-viscosity residue precipitate by adopting a centrifugal separation method to obtain precursor asphalt with low quinoline insoluble substances;
3) adding a modifier into the precursor asphalt, and uniformly stirring to improve the high-temperature rheological property of the precursor asphalt to obtain modified precursor asphalt;
4) cutting the modified precursor asphalt in a pressurized reaction kettle by adopting components to improve the softening point of the modified precursor asphalt; and carrying out vacuum flash evaporation on the modified precursor asphalt subjected to the component cutting treatment to obtain the high-quality high-softening-point coated asphalt for the lithium ion battery cathode material.
The mass fraction of the petroleum asphalt in the mixed asphalt obtained in the step 1) is 20-50%, the stirring temperature is 150-200 ℃, and the stirring time is 1-5 hours.
The organic solvent in the step 2) is a pure solvent or a mixed solvent in toluene, xylene, trimethylbenzene, pentane, hexane, octane, wash oil and kerosene, and the mass ratio of the organic solvent to the mixed asphalt is 1-5: 1.
in the solvent extraction method in the step 2), the stirring temperature of the organic solvent and the mixed asphalt is 150-200 ℃, the stirring time is 1-5 hours, the purification and sedimentation temperature is 150-200 ℃, and the purification and sedimentation time is 1-10 hours.
The centrifugal separation method in the step 2) has the advantages that the rotating speed of the centrifugal machine is 1500-3800 r/min, and the centrifugal time is 1-8 min.
The modifier in the step 3) is naphthenic oil, white mineral oil, paraffin oil or aromatic oil, and the addition amount of the modifier accounts for 3-10% of the mass of the precursor asphalt.
The air flow of the modified precursor asphalt in the step 4) in the pressurized reaction kettle is 0.1-0.5 m3The pressure is 0.2-0.6 MPa, the air stripping time is 3-10 h, and the air stripping temperature is 220-350 ℃.
The temperature of the vacuum flash evaporation is 250-380 ℃, and the vacuum degree is controlled to be 50-100 KPa;
the high-softening-point coated asphalt for the lithium ion battery negative electrode material has a softening point of 150-250 ℃, a quinoline insoluble substance content of less than or equal to 0.3%, a toluene insoluble substance content of 10-45% and a coking value of 50-80%.
Compared with the prior art, the invention has the beneficial effects that:
the medium-temperature coal pitch used as a raw material for preparing the coated pitch has the advantages of high coking value, low price and the like, but the content of quinoline insoluble substances is high, so that the burden of a subsequent treatment process is increased, and the preparation of high-performance coated pitch is not facilitated; the petroleum asphalt used as the raw material of the coating asphalt has the advantages of low sulfur, low impurities and the like, but the price is higher than that of medium-temperature coal asphalt. Therefore, the advantages of the two kinds of asphalt can be integrated by mixing the medium-temperature coal asphalt and the petroleum asphalt as the raw materials of the coated asphalt, and a foundation is laid for preparing the coated asphalt for the high-performance lithium ion battery cathode material. In addition, the modifier is added into the precursor asphalt, so that the flow property of the coated asphalt can be improved, the coated asphalt can repair cracks on the surface of graphite and can also penetrate into the interior of graphite particles to repair pores and holes and the like. In conclusion, the production process is strong in operability, mild in reaction condition and low in cost, the performance of the prepared high-softening-point isotropic coated asphalt completely meets the requirement of the coating process of the lithium ion battery cathode material, the gap in the process is filled, and a strong support is provided for the future development of the graphite carbon cathode material of the lithium ion battery.
Drawings
FIG. 1 is a view showing a structure of a polarized light microscope of coated asphalt obtained in example 1 of the present invention;
FIG. 2 is a view showing a structure of a polarized light microscope of coated asphalt obtained in example 2 of the present invention;
FIG. 3 is a view showing a structure of a polarized light microscope of coated asphalt obtained in example 3 of the present invention;
FIG. 4 is a view showing a structure of a polarized light microscope of coated asphalt obtained in example 4 of the present invention;
FIG. 5 is a scanning electron microscope image of the negative electrode material prepared by coating needle coke with the coated asphalt prepared in example 1 of the present invention;
FIG. 6 is a scanning electron microscope of the negative electrode material prepared by coating needle coke with the coated asphalt in example 2 of the present invention;
FIG. 7 is a scanning electron microscope image of the negative electrode material prepared by coating needle coke with the coated asphalt prepared in example 3 of the present invention;
FIG. 8 is a scanning electron microscope image of the negative electrode material prepared by coating needle coke with the coated asphalt prepared in example 4 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to examples, but the practice of the present invention is not limited to the following embodiments.
The first embodiment is as follows:
respectively weighing 1000g of medium-temperature asphalt and 250g of petroleum asphalt, and uniformly mixing the two kinds of asphalt in a heating reaction kettle at the stirring temperature of 150 ℃ for 2 hours. 1250g of wash oil is added into the composite asphalt at 150 ℃ and continuously stirred for 2h, and after stirring is stopped, the mixture is kept stand for 3h at the constant temperature of 150 ℃, and high-viscosity residue sediment is removed. And (4) placing the residual solution in a centrifuge for secondary purification treatment, wherein the rotation speed of the centrifuge is 2000r/min, and the centrifugation time is 3 min. Adding naphthenic oil modifier accounting for 3% of the mass of the precursor asphalt into the precursor asphalt in a flowing state, uniformly stirring, putting into a pressurized reaction kettle, and air-stripping, wherein the air flow is 0.2m3H, the pressure is 0.2MPa, the stripping time is 6h, and the stripping temperature is 300 ℃. And further improving the softening point of the stripped coated asphalt through vacuum flash evaporation, controlling the flash evaporation temperature at 370 ℃ and the vacuum degree at 80KPa, and removing light components to obtain the high-softening-point coated asphalt. The coated asphalt had a softening point of 193 ℃, a quinoline insoluble content of 0.18%, a toluene insoluble content of 17.14%, and a scorch value of 61.65%, and its polarized light microstructure is shown in FIG. 1. Mixing the pitch with needle cokeCoating the needle coke to prepare a negative electrode material, assembling the negative electrode material into a button lithium ion battery, and performing electrochemical test, wherein the properties of the negative electrode material and the battery test result are shown in table 2 compared with the negative electrode material prepared by non-coating needle coke. The scanning electron microscope picture of the negative electrode material is shown in fig. 5.
The second embodiment:
respectively weighing 1000g of medium-temperature asphalt and 430g of petroleum asphalt, and uniformly mixing the two kinds of asphalt in a heating reaction kettle at the stirring temperature of 150 ℃ for 1.5 h. Adding 1430g of a mixed solvent of wash oil and kerosene into the composite asphalt at 150 ℃, continuously stirring for 2.5h, standing for 4h at the constant temperature of 150 ℃ after stirring is stopped, and removing high-viscosity residue precipitate. And (4) placing the residual solution in a centrifuge for secondary purification treatment, wherein the rotation speed of the centrifuge is 2500r/min, and the centrifugation time is 2 min. Adding paraffin oil modifier with the mass of 3 percent of that of the precursor asphalt into the precursor asphalt in a flowing state, uniformly stirring, and then putting into a pressurized reaction kettle for air lift, wherein the air flow is 0.15m3H, the pressure is 0.3MPa, the stripping time is 4h, and the stripping temperature is 330 ℃. And further improving the softening point of the stripped coated asphalt through vacuum flash evaporation, controlling the flash evaporation temperature at 360 ℃ and the vacuum degree at 85KPa, and removing light components to obtain the high-softening-point coated asphalt. The coated asphalt had a softening point of 185 ℃, a quinoline insoluble content of 0.12%, a toluene insoluble content of 21.25%, a scorch value of 59.83%, and a polarizing microstructure as shown in FIG. 2. The asphalt and the needle coke are coated to prepare a negative electrode material, and the negative electrode material is assembled into a button lithium ion battery for electrochemical test, and compared with the negative electrode material prepared without coating the needle coke, the properties of the negative electrode material and the battery test result are shown in table 2. The scanning electron microscope picture of the negative electrode material is shown in fig. 6.
Example three:
respectively weighing 1000g of medium-temperature asphalt and 670g of petroleum asphalt, and uniformly mixing the two kinds of asphalt in a heating reaction kettle at the stirring temperature of 160 ℃ for 1 h. 2505g of dimethylbenzene is added into the composite asphalt at 160 ℃ to be continuously stirred for 1.5h, and after the stirring is stopped, the mixture is kept stand for 4h at the constant temperature of 160 ℃, so that high-viscosity residue sediment is removed. Putting the residual solution into a centrifuge for secondary purificationAnd (4) performing chemical treatment, wherein the rotating speed of a centrifugal machine is 1800r/min, and the centrifugal time is 4 min. Adding naphthenic oil modifier accounting for 3% of the mass of the precursor asphalt into the precursor asphalt in a flowing state, uniformly stirring, and then putting into a pressurized reaction kettle for air stripping, wherein the air flow is 0.15m3H, the pressure is 0.3MPa, the stripping time is 3h, and the stripping temperature is 310 ℃. And further improving the softening point of the stripped coated asphalt through vacuum flash evaporation, controlling the flash evaporation temperature at 350 ℃ and the vacuum degree at 70KPa, and removing light components to obtain the high-softening-point coated asphalt. The softening point of the coated asphalt was 172 ℃, the quinoline insoluble content was 0.21%, the toluene insoluble content was 15.32%, the scorch value was 56.19%, and the polarizing microstructure thereof was as shown in FIG. 3. The asphalt and the needle coke are coated to prepare a negative electrode material, and the negative electrode material is assembled into a button lithium ion battery for electrochemical test, and compared with the negative electrode material prepared without coating the needle coke, the properties of the negative electrode material and the battery test result are shown in table 2. The scanning electron microscope picture of the negative electrode material is shown in fig. 7.
Example four:
respectively weighing 1000g of medium-temperature asphalt and 670g of petroleum asphalt, and uniformly mixing the two kinds of asphalt in a heating reaction kettle at the stirring temperature of 170 ℃ for 2 hours. Adding 1670g of dimethylbenzene and washing oil mixed solvent into the composite asphalt at 170 ℃, continuously stirring for 1.5h, standing for 5h at the constant temperature of 170 ℃ after stirring is stopped, and removing high-viscosity residue precipitate. And (4) placing the residual solution in a centrifuge for secondary purification treatment, wherein the rotation speed of the centrifuge is 2000r/min, and the centrifugation time is 3 min. Adding naphthenic oil modifier accounting for 3% of the mass of the precursor asphalt into the precursor asphalt in a flowing state, uniformly stirring, and then putting into a pressurized reaction kettle for air lift, wherein the air flow is 0.2m3H, the pressure is 0.4MPa, the stripping time is 6h, and the stripping temperature is 350 ℃. And further increasing the softening point of the stripped coated asphalt through vacuum flash evaporation, controlling the flash evaporation temperature at 370 ℃ and the vacuum degree at 75KPa, and removing light components to obtain the high-softening-point coated asphalt. The coated asphalt had a softening point of 210 ℃, a quinoline insoluble content of 0.16%, a toluene insoluble content of 19.67%, and a scorch value of 63.58%, and its polarized light microstructure is shown in FIG. 4. The pitch is mixed with needle cokeThe cathode material is prepared by coating and assembled into a button lithium ion battery for electrochemical test, and compared with the cathode material prepared by non-coating needle coke, the properties of the cathode material and the battery test result are shown in table 2. The scanning electron microscope picture of the negative electrode material is shown in fig. 8.
TABLE 1 Performance index of the coated asphalts of the examples
TABLE 2 Performance index of negative electrode materials prepared by coating asphalt in examples
The above description is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept within the technical scope of the present invention.
Claims (9)
1. A preparation method of high-softening-point coated asphalt for a lithium ion battery negative electrode material is characterized by comprising the following steps:
1) taking medium-temperature coal pitch as a raw material, adding petroleum pitch into the medium-temperature coal pitch, and uniformly mixing the two kinds of pitch in a reaction kettle with a heating and stirring device to prepare mixed pitch;
2) adding an organic solvent into the mixed asphalt by adopting a solvent extraction method to remove high-viscosity residue precipitate, and performing primary purification treatment; performing secondary purification treatment on the mixed asphalt without the high-viscosity residue precipitate by adopting a centrifugal separation method to obtain precursor asphalt with low quinoline insoluble substances;
3) adding a modifier into the precursor asphalt, and uniformly stirring to improve the high-temperature rheological property of the precursor asphalt to obtain modified precursor asphalt;
4) cutting the modified precursor asphalt in a pressurized reaction kettle by adopting components to improve the softening point of the modified precursor asphalt; and carrying out vacuum flash evaporation on the modified precursor asphalt subjected to the component cutting treatment to obtain the high-softening-point coated asphalt for the lithium ion battery cathode material.
2. The preparation method of the high-softening-point coated asphalt for the lithium ion battery negative electrode material according to claim 1, wherein the mass fraction of the petroleum asphalt in the mixed asphalt in the step 1) is 20-50%, the stirring temperature is 150-200 ℃, and the stirring time is 1-5 hours.
3. The preparation method of the high-softening-point coated asphalt for the lithium ion battery negative electrode material according to claim 1, wherein the organic solvent in the step 2) is a pure solvent or a mixed solvent of toluene, xylene, trimethylbenzene, pentane, hexane, octane, wash oil and kerosene, and the mass ratio of the organic solvent to the mixed asphalt is 1-5: 1.
4. the method for preparing the high-softening-point coated asphalt for the lithium ion battery negative electrode material according to claim 1 or 3, wherein in the solvent extraction method in the step 2), the stirring temperature of the organic solvent and the mixed asphalt is 150-200 ℃, the stirring time is 1-5 hours, the purification and sedimentation temperature is 150-200 ℃, and the purification and sedimentation time is 1-10 hours.
5. The method for preparing the high-softening-point coated asphalt for the lithium ion battery anode material according to claim 1, wherein the centrifugal separation method in the step 2) is performed at a centrifuge rotation speed of 1500-3800 r/min for 1-8 min.
6. The method for preparing the high-softening-point coated asphalt for the lithium ion battery negative electrode material according to claim 1, wherein the modifier in the step 3) is naphthenic oil, white mineral oil, paraffin oil or aromatic oil, and the addition amount of the modifier accounts for 3-10% of the mass of the precursor asphalt.
7. The method for preparing the high-softening-point coated asphalt for the lithium ion battery negative electrode material according to claim 1, wherein the air flow rate of the modified precursor asphalt in the step 4) in the pressurized reaction kettle is 0.1-0.5 m3The pressure is 0.2-0.6 MPa, the air stripping time is 3-10 h, and the air stripping temperature is 220-350 ℃.
8. The preparation method of the high-softening-point coated asphalt for the lithium ion battery negative electrode material according to claim 1 or 7, characterized in that the temperature of vacuum flash evaporation is 250-380 ℃, and the vacuum degree is controlled at 50-100 KPa.
9. The preparation method of the high-softening-point coated asphalt for the lithium ion battery negative electrode material according to claim 1, wherein the high-softening-point coated asphalt for the lithium ion battery negative electrode material has a softening point of 150-250 ℃, a quinoline insoluble content of 0.3% or less, a toluene insoluble content of 10-45%, and a coking value of 50-80%.
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