CN112537765B - Preparation method of lithium ion battery carbon negative electrode material - Google Patents
Preparation method of lithium ion battery carbon negative electrode material Download PDFInfo
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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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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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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Abstract
The invention relates to preparation of a battery cathode material, and aims to provide a preparation method of a carbon cathode material of a lithium ion battery. The method specifically comprises the following steps: freeze-drying fresh peanut shells to obtain dried peanut shells; dipping in liquid paraffin at 200 ℃, taking out and drying to obtain a preliminarily reconstructed peanut shell; soaking in ricinoleic acid at 100 deg.C, taking out, and drying; then immersing the peanut shells into hydrogen peroxide solution for hydrothermal treatment to obtain second reconstructed peanut shells; grinding and mixing with sodium trifluorobenzene sulfonate uniformly; burning the mixture under the protection of nitrogen; and cooling to room temperature to obtain the carbon cathode material of the lithium ion battery. The cathode material obtained by the invention has high charge-discharge cycle stability, and is a carbon cathode material with wide source and low cost. The charging and discharging times of the prepared carbon cathode material can reach more than 10000, and a new preparation process of the lithium ion battery is developed.
Description
Technical Field
The invention relates to preparation of a battery material, in particular to a preparation method of a carbon negative electrode material of a lithium battery.
Background
The global lithium battery cathode material sales amount is about more than ten thousand tons, and the demand for the cathode material is in a continuously increasing state according to the increasing trend of new energy automobiles at the present stage. At present, natural/artificial graphite is still the main negative electrode material of lithium batteries in the world, and other novel negative electrode carbon materials are also in rapid growth. As a negative electrode material, graphite has many disadvantages, such as low potential of graphite, formation of an interface film with an electrolyte, and easy occurrence of lithium precipitation; the ion migration speed is low, so the charge-discharge multiplying power is low; the graphite having a layered structure is deformed by about 10% during the insertion and extraction of lithium ions, affecting the cycle life of the battery.
Soft carbon (i.e., easily graphitizable carbon) refers to amorphous carbon that can be graphitized at a temperature of 2000 ℃ or higher, and petroleum coke, needle coke, and the like are common. The electrolyte has low crystallinity, small crystal grain size, larger crystal face spacing and good compatibility with the electrolyte. But the first charge and discharge irreversible capacity is high, the output voltage is lower, and the negative electrode material is not directly used generally.
Hard carbon (hard carbon), also known as non-graphitizable carbon, is a pyrolytic carbon of high molecular polymers, which is also non-graphitizable at high temperatures of 3000 ℃. Hard carbons include resin carbons (e.g., phenol resin, epoxy resin, polyfurfuryl alcohol, etc.), organic polymer pyrolytic carbons (PVA, PVC, PVDF, PAN, etc.), carbon black (acetylene black); is beneficial to the insertion of lithium without causing the obvious expansion of the structure and has good charge-discharge cycle performance. However, the irreversible capacity of hard carbon is too large, which is not favorable for improving the performance of the lithium ion battery.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a carbon cathode material of a lithium ion battery.
In order to solve the technical problem, the solution of the invention is as follows:
the preparation method of the carbon cathode material of the lithium ion battery comprises the following steps:
(1) Freeze-drying the cleaned fresh peanut shells to constant weight to obtain dried peanut shells;
(2) Immersing the dried peanut shells into liquid paraffin at the temperature of 200 ℃, and taking out after 12-36 hours; spin-drying redundant liquid paraffin on the surface of the peanut shell to obtain a primarily reconstructed peanut shell;
(3) Immersing the primarily reconstructed peanut shells into ricinoleic acid at 100 ℃, taking out the peanut shells after 4 to 6 hours, and spin-drying the redundant ricinoleic acid on the surfaces of the peanut shells; then immersing the peanut shells into a hydrogen peroxide solution, uniformly mixing, adding the mixture into a hydrothermal kettle, and carrying out hydrothermal treatment at 140 ℃ for 4-6 hours to obtain second reconstructed peanut shells;
(3) Grinding the peanut shells reconstructed for the second time until the average grain diameter is less than 100 microns, and then uniformly mixing the ground peanut shells with sodium trifluorobenzene sulfonate according to the mass ratio of 1: 0.03; heating the mixture to 400-600 ℃ under the protection of nitrogen, and preserving the heat for 4-6 hours; and cooling to room temperature to obtain the lithium ion battery carbon negative electrode material.
In the invention, in the step (3), the mass percentage concentration of the hydrogen peroxide solution is 20%, and the mass ratio of the peanut shells to the hydrogen peroxide is 1: 30.
The carbon cathode material obtained by the invention is used for preparing the lithium ion battery cathode, and when the cathode is used for further assembling the lithium ion battery, the conventional technology is adopted, and the invention has no special requirement.
Description of the inventive principles:
at present, no relevant documents describe the use of fruit shells for the preparation of anode materials. The inventor finds that the cathode material can be reconstructed by using the peanut shells, and the cellulose cross-linked structure is more compact in the process, so that the final cathode material has better cycle stability. Through a large number of experiments, the inventors compare the anode materials obtained by using a large number of cellulose sources including walnut shells, sunflower seed shells, corncobs and the like, and find that the anode materials obtained by reconstructing peanut shells have the optimal performance.
Compared with the prior art, the invention has the following beneficial effects:
1. the cathode material obtained by the invention has high charge-discharge cycle stability, and is a carbon cathode material with wide source and low cost.
2. The charging and discharging times of the carbon cathode material prepared by the method can reach more than 10000, and a novel lithium ion battery preparation process is developed.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1:
a preparation method of a carbon cathode material of a lithium ion battery comprises the following steps:
(1) And (3) cleaning and freeze-drying the fresh peanut shells to constant weight to obtain the dried peanut shells.
(2) And (2) immersing the dried peanut shells obtained in the step (1) into liquid paraffin at the temperature of 200 ℃, taking out the dried peanut shells after 12 hours, and spin-drying the redundant liquid paraffin on the surfaces of the peanut shells to obtain the primarily reconstructed peanut shells.
(3) Immersing the primarily reconstructed peanut shells obtained in the step (2) into ricinoleic acid at 100 ℃, taking out after 4 hours, spin-drying redundant ricinoleic acid on the surfaces of the peanut shells, and immersing the peanut shells into hydrogen peroxide solution with the mass percentage concentration of 20% (the mass ratio of the peanut shells to the hydrogen peroxide solution is 1; and adding the mixture into a 500ml hydrothermal kettle, and carrying out hydrothermal treatment at 140 ℃ for 4 hours to obtain the second reconstructed peanut shells.
(3) Grinding the peanut shells reconstructed for the second time in the step (3) until the average particle size is smaller than 100 micrometers, and mixing the ground peanut shells with sodium trifluorobenzene sulfonate in a mass ratio of 1:0.03, heating the mixture to 400 ℃ under the protection of nitrogen, preserving the heat for 4 hours, and cooling to room temperature to obtain the carbon cathode material of the lithium ion battery.
(4) The lithium ion battery was assembled as follows:
preparation of negative electrode (method of using negative electrode material): mixing a negative electrode material and carboxymethyl fibers in a mass ratio of 9:1, mixing and pressing into pole pieces.
Preparing an anode: taking commercially available lithium iron phosphate, and mixing the lithium iron phosphate with carboxymethyl fibers according to a mass ratio of 9:1, mixing and pressing into pole pieces.
Preparing electrolyte: conventional commercial electrolytes for lithium ion batteries.
Assembling the lithium ion battery: and flatly placing the negative electrode shell on the insulating table top, placing the metal lithium sheet in the center of the negative electrode shell, flattening the metal lithium sheet by using a sheet pressing mold, flatly placing the diaphragm on the upper layer of the lithium sheet, and dropwise adding a proper amount of electrolyte on the surface of the diaphragm by using a liquid transfer machine. And (4) placing the test pole piece, the gasket, the spring piece and the positive shell on the upper layer of the diaphragm in sequence by using insulating tweezers. And further, placing the negative electrode side of the button cell on a button cell sealing machine die upwards by using insulating tweezers, using a paper towel to be padded above the cell to absorb overflowed electrolyte, adjusting the pressure to 800Pa to press for 5s to complete assembly and prepare the button cell, taking out the button cell by using the insulating tweezers, observing whether the prepared appearance is complete and wiping the button cell completely by using the paper towel.
The lithium ion battery using the carbon negative electrode material prepared in this example was subjected to a charge/discharge test in accordance with the test method specified in GJB 4477-2004, and the number of charge/discharge times reached 11000 times.
Example 2:
a preparation method of a carbon cathode material of a lithium ion battery comprises the following steps:
(1) And (3) cleaning and freeze-drying the fresh peanut shells to constant weight to obtain the dried peanut shells.
(2) And (2) immersing the dried peanut shells obtained in the step (1) in liquid paraffin at 200 ℃, taking out after 36 hours, and spin-drying redundant liquid paraffin on the surfaces of the peanut shells to obtain the preliminarily reconstructed peanut shells.
(3) Immersing the primarily reconstructed peanut shells obtained in the step (2) into ricinoleic acid at 100 ℃, taking out after 6 hours, spin-drying redundant ricinoleic acid on the surfaces of the peanut shells, and immersing the peanut shells into hydrogen peroxide solution with the mass percentage concentration of 20% (the mass ratio of the peanut shells to the hydrogen peroxide solution is 1; and adding the mixture into a 500ml hydrothermal kettle, and carrying out hydrothermal treatment at 140 ℃ for 6 hours to obtain the second reconstructed peanut shells.
(3) Grinding the peanut shells reconstructed for the second time in the step (3) until the average particle size is smaller than 100 micrometers, and mixing the ground peanut shells with sodium trifluorobenzene sulfonate in a mass ratio of 1:0.03, heating the mixture to 600 ℃ under the protection of nitrogen, preserving the heat for 6 hours, and cooling to room temperature to obtain the carbon cathode material of the lithium ion battery.
(4) The lithium ion battery assembly and test work is carried out according to the method in the step (4) in the example 1, and the charging and discharging times of the carbon negative electrode material obtained in the example can reach 14600 times.
Example 3:
a preparation method of a carbon cathode material of a lithium ion battery comprises the following steps:
(1) And (3) cleaning and freeze-drying the fresh peanut shells to constant weight to obtain the dried peanut shells.
(2) And (2) immersing the dried peanut shells obtained in the step (1) into liquid paraffin at the temperature of 200 ℃, taking out the dried peanut shells after 24 hours, and spin-drying the redundant liquid paraffin on the surfaces of the peanut shells to obtain the primarily reconstructed peanut shells.
(3) Immersing the primarily reconstructed peanut shells obtained in the step (2) into ricinoleic acid at 100 ℃, taking out after 5 hours, spin-drying redundant ricinoleic acid on the surfaces of the peanut shells, and immersing the peanut shells into hydrogen peroxide solution with the mass percentage concentration of 20% (the mass ratio of the peanut shells to the hydrogen peroxide solution is 1; and adding the mixture into a 500ml hydrothermal kettle, and carrying out hydrothermal treatment at 140 ℃ for 5 hours to obtain the second reconstructed peanut shells.
(3) Grinding the peanut shells reconstructed for the second time in the step (3) until the average particle size is smaller than 100 micrometers, and mixing the ground peanut shells with sodium trifluorobenzene sulfonate in a mass ratio of 1:0.03, heating the mixture to 500 ℃ under the protection of nitrogen, preserving the heat for 5 hours, and cooling to room temperature to obtain the carbon cathode material of the lithium ion battery.
(4) The lithium ion battery assembly and test work is carried out according to the method in the step (4) in the embodiment 1, and the charging and discharging times of the carbon negative electrode material obtained in the embodiment can reach 15500 times.
Comparative example 1
The lithium ion battery was assembled as follows:
preparation of negative electrode (method of using negative electrode material): mixing graphite and carboxymethyl fiber in a mass ratio of 9:1, mixing and pressing into pole pieces.
Preparing an anode: taking commercially available lithium iron phosphate, and mixing the lithium iron phosphate with the carboxymethyl fibers in a mass ratio of 9:1, mixing and pressing into pole pieces.
Preparing electrolyte: conventional commercial electrolytes for lithium ion batteries.
Assembling and testing the lithium ion battery:
and flatly placing the negative electrode shell on the insulating table top, placing the metal lithium sheet in the center of the negative electrode shell, flattening the metal lithium sheet by using a sheet pressing mold, flatly placing the diaphragm on the upper layer of the lithium sheet, and dropwise adding a proper amount of electrolyte on the surface of the diaphragm by using a liquid transfer machine. And (4) placing the test pole piece, the gasket, the spring piece and the positive shell on the upper layer of the diaphragm in sequence by using insulating tweezers. And further, placing the negative electrode side of the button cell on a button cell sealing machine die upwards by using insulating tweezers, using a paper towel to be padded above the cell to absorb overflowed electrolyte, adjusting the pressure to 800Pa to press for 5s to complete assembly and prepare the button cell, taking out the button cell by using the insulating tweezers, observing whether the prepared appearance is complete and wiping the button cell completely by using the paper towel.
The lithium ion battery using the carbon negative electrode material prepared in this example was subjected to a charge/discharge test in accordance with the test method specified in GJB 4477-2004, and the number of charge/discharge cycles was 5500.
Comparative example 2
The lithium ion battery was assembled as follows:
preparation of negative electrode (method of using negative electrode material): mixing polysilicon with carboxymethyl fiber according to a mass ratio of 9:1, mixing and pressing into pole pieces.
Preparing an anode: taking commercially available lithium iron phosphate, and mixing the lithium iron phosphate with the carboxymethyl fibers in a mass ratio of 9:1, mixing and pressing into pole pieces.
Preparing electrolyte: conventional commercial electrolytes for lithium ion batteries.
Assembling and testing the lithium ion battery:
and flatly placing the negative electrode shell on the insulating table board, placing the metal lithium sheet in the center of the negative electrode shell, flattening the metal lithium sheet by using a sheet pressing mold, flatly placing the diaphragm on the upper layer of the lithium sheet, and dropwise adding a proper amount of electrolyte on the surface of the diaphragm by using a pipettor. And (4) placing the test pole piece, the gasket, the spring piece and the positive shell on the upper layer of the diaphragm in sequence by using insulating tweezers. And further, placing the negative electrode side of the button cell on a button cell sealing machine die upwards by using insulating tweezers, using a paper towel to be padded above the cell to absorb overflowed electrolyte, adjusting the pressure to 800Pa to press for 5s to complete assembly and prepare the button cell, taking out the button cell by using the insulating tweezers, observing whether the prepared appearance is complete and wiping the button cell completely by using the paper towel.
The charging and discharging tests were carried out according to the test method specified in GJB 4477-2004, and the number of charging and discharging times of the lithium ion battery using the carbon negative electrode material prepared in this example can reach 3500.
Compared with comparative examples 1 and 2, the anodes, the electrolyte and the battery assembly operation method used in the assembly process of the lithium ion batteries in the above examples 1 to 3 are consistent, and the only difference is that the cathodes made of different materials are used. According to the charge and discharge test results of the lithium ion battery, the negative electrode prepared from the carbon negative electrode material prepared by the method has obvious influence on the improvement of the charge and discharge performance of the lithium ion battery; can greatly improve the cycle period and prolong the service life of the product.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (1)
1. A preparation method of a carbon cathode material of a lithium ion battery is characterized by comprising the following steps:
(1) Freeze-drying the cleaned fresh peanut shells to constant weight to obtain dried peanut shells;
(2) Immersing the dried peanut shells into liquid paraffin at the temperature of 200 ℃, and taking out after 12 to 36 hours; spin-drying redundant liquid paraffin on the surface of the peanut shell to obtain a primarily reconstructed peanut shell;
(3) Immersing the preliminarily reconstructed peanut shells into ricinoleic acid at the temperature of 100 ℃, taking out the peanut shells after 4 to 6 hours, and spin-drying redundant ricinoleic acid on the surfaces of the peanut shells; then immersing the peanut shells into a hydrogen peroxide solution, uniformly mixing, adding the mixture into a hydrothermal kettle, and carrying out hydrothermal treatment at 140 ℃ for 4-6 hours to obtain second-time reconstructed peanut shells; the mass percentage concentration of the hydrogen peroxide solution is 20 percent, and the mass ratio of the peanut shells to the hydrogen peroxide is 1: 30;
(4) Grinding the peanut shells reconstructed for the second time until the average particle size is less than 100 micrometers, and then uniformly mixing the ground peanut shells with sodium trifluorobenzene sulfonate according to the mass ratio of 1: 0.03; heating the mixture to 400-600 ℃ under the protection of nitrogen, and preserving heat for 4-6 hours; and cooling to room temperature to obtain the carbon cathode material of the lithium ion battery.
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