CN114335476A - Preparation method and application of negative electrode material - Google Patents
Preparation method and application of negative electrode material Download PDFInfo
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Abstract
The invention relates to the technical field of batteries, in particular to a preparation method and application of a negative electrode material. The preparation method of the anode material provided by the invention comprises the following steps: dissolving naphthalene tetracarboxylic dianhydride and aminosalicylic acid in a first solvent, and heating for reaction to obtain a ligand product; dissolving the ligand product and metal salt in a second solvent, and heating for reaction to obtain a metal MOF product; and dissolving the metal MOF product and graphite oxide in a third solvent, and heating for reaction to obtain the negative electrode material. The negative electrode material prepared by the preparation method provided by the invention can well relieve the volume expansion phenomenon in the charging and discharging process, meanwhile, the introduction of graphite oxide can effectively improve the conductivity of the electrode material, and the porous structure of the MOF can improve a channel for lithium ion transmission, thereby showing excellent electrochemical performance and cycle performance.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a preparation method and application of a negative electrode material.
Background
Due to the continuous consumption of traditional fossil fuels and global environmental concerns, there is increasing interest in developing sustainable clean energy. Secondary batteries have become one of the most promising energy storage devices due to their high energy conversion efficiency and portability. Among them, the lithium ion battery has the advantages of high energy density, low self-discharge rate, long cycle life, light weight and the like, and is widely applied to the fields of automobiles, electric tools, energy storage and the like.
Commercial lithium ion batteries consist of a positive electrode material, a negative electrode material, a separator and an electrolyte. The common cathode material is graphite, which has a stable structure, good conductivity and safety. However, the theoretical specific capacity of the graphite is only 372mAh/g, the solid-state electron diffusion capacity of the graphite is poor, and the demand of people for high-power and high-energy-density batteries in the future cannot be met. When the traditional MOF materials such as silicon-based materials, nickel-based materials and the like are used as the negative electrode materials of the lithium ion batteries, the high theoretical specific capacity is shown, but the traditional MOF materials have poor conductivity and serious volume expansion phenomena in the circulating process, so that the circulating performance of the traditional MOF materials is greatly limited, and the practical application of the materials is influenced.
Disclosure of Invention
The invention aims to overcome the defects that in the prior art, a metal MOF material has poor conductivity and serious volume expansion phenomenon in a circulation process so as to limit the circulation performance of the metal MOF material, and further provides a preparation method and application of a negative electrode material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of the anode material comprises the following steps:
1) dissolving naphthalene tetracarboxylic dianhydride and aminosalicylic acid in a first solvent, and heating for reaction to obtain a ligand product;
2) dissolving the ligand product and metal salt in a second solvent, and heating for reaction to obtain a metal MOF product;
3) and dissolving the metal MOF product and graphite oxide in a third solvent, and heating for reaction to obtain the negative electrode material.
Preferably, in the step 1), the molar ratio of the naphthalene tetracarboxylic dianhydride to the aminosalicylic acid is 1: (1.1-2), the heating reaction temperature is 120-150 ℃, and the heating reaction time is 12-48 h;
in the step 2), the molar ratio of the ligand product to the metal salt is 1: (2-2.5), the heating reaction temperature is 120-150 ℃, and the heating reaction time is 24-48 h;
in the step 3), the adding amount of the graphite oxide is 0.1-50% of the mass of the metal MOF product, the heating reaction temperature is 150-180 ℃, and the heating reaction time is 12-48 h.
Preferably, the step 2) further comprises the steps of filtering, washing and freeze-drying the reaction solution after the heating reaction is finished;
and 3) after the heating reaction is finished, filtering, washing and freeze-drying the reaction liquid.
Preferably, the washing step in the step 2) is carried out by sequentially washing with N, N-dimethylformamide, ethanol and water, wherein the freeze-drying temperature is-30 to-40 ℃ and the freeze-drying time is 24 to 48 hours.
And in the step 3), the washing step adopts deionized water for washing, the freeze-drying temperature is-30-40 ℃, and the freeze-drying time is 24-48 h.
Preferably, the step 1) further comprises the steps of filtering, washing and drying the reaction solution after the heating reaction is finished.
Preferably, in the step 1), the washing step adopts N, N-dimethylformamide, diethyl ether and methanol to wash sequentially, the drying is vacuum drying, the drying temperature is 80-100 ℃, and the drying time is 24-48 h.
Preferably, the heating reaction in step 1) is carried out under the protection of nitrogen or inert gas; further comprising the step of purifying the ligand product. Preferably, the ligand product is purified using hydrochloric acid, optionally at a concentration of 1 to 3 mol/L.
Preferably, the first solvent and the second solvent are both N, N-dimethylformamide, and the third solvent is water;
the metal salt is metal nitrate and is selected from at least one of copper nitrate, nickel nitrate and cobalt nitrate.
The naphthalene tetracarboxylic dianhydride is 1,4,5, 8-naphthalene tetracarboxylic anhydride, and the aminosalicylic acid can be p-aminosalicylic acid or 3-aminosalicylic acid.
Preferably, after the naphthalene tetracarboxylic dianhydride and the aminosalicylic acid are added into the first solvent in the step 1), in order to ensure uniform dispersion, the method further comprises the step of performing ultrasonic dispersion on the mixed solution, optionally, the ultrasonic power is 120W-180W, and the ultrasonic time is 30-60 min. Optionally, the amount of the first solvent added is 20-40 mL.
Preferably, after the ligand product and the metal salt are added into the second solvent in step 2), in order to ensure uniform dispersion, the method further comprises a step of performing ultrasonic dispersion on the mixed solution, optionally, the ultrasonic power is 120W-180W, and the ultrasonic time is 30-60 min. Optionally, the second solvent is added in an amount of 8-15 mL.
Preferably, after the metal MOF product and the graphite oxide are added into the third solvent in step 3), in order to ensure uniform dispersion, the method further comprises the step of performing ultrasonic dispersion on the mixed solution, optionally, the ultrasonic power is 120W-180W, and the ultrasonic time is 30-60 min. Optionally, the amount of the third solvent added is 10-15 mL.
The invention also provides a negative plate which comprises a current collector and a negative material on the current collector, wherein the negative material is prepared by the preparation method.
The invention also provides a lithium ion battery which comprises a positive plate and a negative plate, wherein the negative plate is the negative plate.
The invention has the beneficial effects that:
1. according to the preparation method of the negative electrode material, the naphthalene tetracarboxylic dianhydride and the aminosalicylic acid are heated to react to form a specific grafting ligand structure (the grafting ligand structure retains hydroxyl and carboxyl functional groups of the aminosalicylic acid and can be well complexed with metal ions), then the specific ligand and the metal salt are compounded, the obtained metal MOF product is further reacted with graphite oxide, and the obtained composite material has a rich pore structure and a large specific surface area, and can well relieve the volume expansion phenomenon in the charging and discharging processes when being used as the negative electrode material. Meanwhile, the introduction of graphite oxide can effectively improve the conductivity of the electrode material, and the porous structure of the MOF can improve a channel for lithium ion transmission, so that excellent electrochemical performance and cycle performance are shown.
The negative electrode material prepared by the preparation method provided by the invention is compounded with metal salt through a specific ligand, and then is compounded with graphite oxide, so that the obtained electrode material has good conductivity and porous structure, can provide a large number of active sites for lithium ions, and shows excellent electrochemical performance and cycle performance when being used as a negative electrode material of a lithium ion battery.
2. The preparation method of the negative electrode material provided by the invention further adopts a freeze-drying method to freeze-dry the product in the step 2) and the step 3) to better stabilize the MOF structure, so that the MOF structure can keep rich pore structures and larger specific surface area, and the MOF structure is more favorable for relieving the volume expansion phenomenon in the charge-discharge process when being used as an electrode material, so that the MOF structure shows excellent electrochemical performance and cycle performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is an SEM electron micrograph of the anode material prepared in example 1 of the present invention.
FIG. 2 is a cycle performance curve of a CR2025 button cell prepared by using the negative electrode material of example 1 of the present invention at a current density of 50 mA/g;
FIG. 3 is a cycle performance curve of a CR2025 button cell prepared by using the negative electrode material of example 1 of the present invention at a current density of 2000 mA/g;
fig. 4 is a cycling curve of CR2025 button cell prepared from the negative electrode material of example 1 under different current densities.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
The embodiment provides a preparation method of an anode material, which comprises the following steps:
1) adding 35mmol of naphthalene tetracarboxylic dianhydride and 70mmol of p-aminosalicylic acid into 30mL of N, N-Dimethylformamide (DMF), performing ultrasonic treatment for 60min at 120W by using an ultrasonic cleaner to uniformly disperse the solution, transferring the solution into a reaction kettle under the protection of nitrogen to react for 24h at 130 ℃, after the reaction is finished, cooling the reaction kettle to room temperature, filtering the obtained yellow suspension reaction solution, sequentially washing a filter cake by using DMF, diethyl ether and methanol, after the washing is finished, putting the washed filter cake into an oven to perform vacuum drying at 100 ℃, wherein the drying time is 24h to obtain yellow powder, and purifying the obtained yellow powder by using hydrochloric acid (the concentration of hydrochloric acid is 2mol/L) by using a Soxhlet extractor to obtain a ligand product;
2) mixing copper nitrate and the ligand product obtained in the step 1) (the mass ratio of the copper nitrate to the ligand product is 2: 1) adding the solution into 8mL of DMF, performing ultrasonic treatment for 60min at 120W, transferring the solution into a reaction kettle, reacting for 24h at 120 ℃, after the reaction is finished, cooling the reaction kettle to room temperature, filtering the obtained reaction solution, sequentially washing a filter cake with DMF, ethanol and deionized water, and freeze-drying the filter cake in a freeze-drying machine at-35 ℃ for 24h to obtain a CuMOF product;
3) adding the CuMOF product obtained in the step 2) and brown graphite oxide (the adding amount of the graphite oxide is 20% of the mass of the CuMOF product) into 15mL of deionized water, performing ultrasonic treatment for 1h under 120W, transferring the solution into a reaction kettle, performing reaction for 24h at 180 ℃, after the reaction is finished, cooling the reaction kettle to room temperature, filtering the obtained reaction solution, washing a filter cake with deionized water, freeze-drying the filter cake in a freeze-drying machine after the washing is finished, wherein the freeze-drying temperature is-35 ℃, and the freeze-drying time is 24h, so as to obtain the cathode material.
Example 2
The embodiment provides a preparation method of an anode material, which comprises the following steps:
1) adding 35mmol of naphthalene tetracarboxylic dianhydride and 70mmol of p-aminosalicylic acid into 30mL of N, N-Dimethylformamide (DMF), performing ultrasonic treatment for 60min at 120W by using an ultrasonic cleaner to uniformly disperse the solution, transferring the solution into a reaction kettle under the protection of nitrogen to react for 24h at 130 ℃, after the reaction is finished, cooling the reaction kettle to room temperature, filtering the obtained yellow suspension reaction solution, sequentially washing a filter cake by using DMF, diethyl ether and methanol, after the washing is finished, putting the washed filter cake into an oven to perform vacuum drying at 100 ℃, wherein the drying time is 24h to obtain yellow powder, and purifying the obtained yellow powder by using hydrochloric acid (the concentration of hydrochloric acid is 2mol/L) by using a Soxhlet extractor to obtain a ligand product;
2) mixing copper nitrate and the ligand product obtained in the step 1) (the mass ratio of the copper nitrate to the ligand product is 2: 1) adding the solution into 8mL of DMF, performing ultrasonic treatment for 60min at 120W, transferring the solution into a reaction kettle, reacting for 24h at 120 ℃, after the reaction is finished, cooling the reaction kettle to room temperature, filtering the obtained reaction solution, sequentially washing a filter cake with DMF, ethanol and deionized water, and freeze-drying the filter cake in a freeze-drying machine at-35 ℃ for 24h to obtain a CuMOF product;
3) adding the CuMOF product obtained in the step 2) and brown graphite oxide (the adding amount of the graphite oxide is 10% of the mass of the CuMOF product) into 15mL of deionized water, performing ultrasonic treatment for 1h under 120W, transferring the solution into a reaction kettle, performing reaction for 24h at 180 ℃, after the reaction is finished, cooling the reaction kettle to room temperature, filtering the obtained reaction solution, washing a filter cake with deionized water, freeze-drying the filter cake in a freeze-drying machine after the washing is finished, wherein the freeze-drying temperature is-35 ℃, and the freeze-drying time is 24h, so as to obtain the cathode material.
Example 3
The embodiment provides a preparation method of an anode material, which comprises the following steps:
1) adding 35mmol of naphthalene tetracarboxylic dianhydride and 70mmol of p-aminosalicylic acid into 30mL of N, N-Dimethylformamide (DMF), performing ultrasonic treatment for 60min at 120W by using an ultrasonic cleaner to uniformly disperse the solution, transferring the solution into a reaction kettle under the protection of nitrogen to react for 24h at 130 ℃, after the reaction is finished, cooling the reaction kettle to room temperature, filtering the obtained yellow suspension reaction solution, sequentially washing a filter cake by using DMF, diethyl ether and methanol, after the washing is finished, putting the washed filter cake into an oven to perform vacuum drying at 100 ℃, wherein the drying time is 24h to obtain yellow powder, and purifying the obtained yellow powder by using hydrochloric acid (the concentration of hydrochloric acid is 2mol/L) by using a Soxhlet extractor to obtain a ligand product;
2) mixing copper nitrate and the ligand product obtained in the step 1) (the mass ratio of the copper nitrate to the ligand product is 2: 1) adding the solution into 8mL of DMF, performing ultrasonic treatment for 60min at 120W, transferring the solution into a reaction kettle, reacting for 24h at 120 ℃, after the reaction is finished, cooling the reaction kettle to room temperature, filtering the obtained reaction solution, sequentially washing a filter cake with DMF, ethanol and deionized water, and freeze-drying the filter cake in a freeze-drying machine at-35 ℃ for 24h to obtain a CuMOF product;
3) adding the CuMOF product obtained in the step 2) and brown graphite oxide (the adding amount of the graphite oxide is 50% of the mass of the CuMOF product) into 15mL of deionized water, performing ultrasonic treatment for 1h under 120W, transferring the solution into a reaction kettle, performing reaction for 24h at 180 ℃, after the reaction is finished, cooling the reaction kettle to room temperature, filtering the obtained reaction solution, washing a filter cake with deionized water, freeze-drying the filter cake in a freeze-drying machine after the washing is finished, wherein the freeze-drying temperature is-35 ℃, and the freeze-drying time is 24h, so as to obtain the cathode material.
Comparative example 1
This comparative example provides a method for preparing a negative electrode material, which is different from example 1 in that naphthalene tetracarboxylic dianhydride is replaced with 1, 8-naphthalic anhydride in step 1).
Comparative example 2
This comparative example provides a method for preparing a negative electrode material, which is different from example 1 in that p-aminosalicylic acid is replaced with p-aminobenzoic acid in step 1).
Comparative example 3
The comparative example provides a preparation method of a negative electrode material, and the difference between the preparation method and the example 1 is that after washing in the step 2), a filter cake is placed into an oven for vacuum drying, the drying temperature is 100 ℃, and the drying time is 24 hours, so that a CuMOF product is obtained;
and 3) after washing in the step 3), putting the filter cake into an oven for vacuum drying, wherein the drying temperature is 100 ℃, and the drying time is 24 hours, so as to obtain the cathode material.
Test example 1
The negative electrode materials prepared in the above examples and comparative examples and the CuMOF product prepared in example 1 were assembled into a lithium ion battery, and a charge and discharge test was performed, specifically as follows:
respectively mixing the cathode material or the CuMOF product prepared in example 1 with acetylene black and PVDF (polyvinylidene fluoride) according to a mass ratio of 8: 1:1, coating the mixture on a copper foil, performing vacuum drying and rolling, cutting an electrode material into a round disc with the diameter of 12mm by using a round punching machine to be used as a negative electrode of a lithium ion battery, using a lithium sheet as a positive electrode of lithium ions, adopting a Celgard2400 porous polypropylene film as a diaphragm, using a mixed solution (the volume ratio of EC, DMC and DEC is 1:1:1) containing 1mol/L of LiPF6 EC (ethylene carbonate), DMC (dimethyl carbonate) and DEC (diethyl carbonate) as an electrolyte, and finally assembling the mixture in a glove box filled with argon to obtain the CR2025 button cell. The first discharge capacity and the specific capacity of the assembled battery under the current density of 50mA/g of the battery are tested under the conditions that the temperature is 25 ℃ and the voltage is 0.01-3V, and the coulomb efficiency of the assembled battery is tested after the assembled battery is circulated for 80 times under the current density of 50mA/g within the voltage range of 0.01-3V. The test results are shown in table 1.
TABLE 1
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The preparation method of the anode material is characterized by comprising the following steps of:
1) dissolving naphthalene tetracarboxylic dianhydride and aminosalicylic acid in a first solvent, and heating for reaction to obtain a ligand product;
2) dissolving the ligand product and metal salt in a second solvent, and heating for reaction to obtain a metal MOF product;
3) and dissolving the metal MOF product and graphite oxide in a third solvent, and heating for reaction to obtain the negative electrode material.
2. The method for preparing the negative electrode material according to claim 1, wherein in the step 1), the molar ratio of the naphthalene tetracarboxylic dianhydride to the aminosalicylic acid is 1: (1.1-2), the heating reaction temperature is 120-150 ℃, and the heating reaction time is 12-48 h;
in the step 2), the mass ratio of the ligand product to the metal salt is 1: (2-2.5), the heating reaction temperature is 120-150 ℃, and the heating reaction time is 24-48 h;
in the step 3), the adding amount of the graphite oxide is 0.1-50% of the mass of the metal MOF product, the heating reaction temperature is 150-180 ℃, and the heating reaction time is 12-48 h.
3. The preparation method of the anode material according to claim 1 or 2, wherein the step 2) further comprises the steps of filtering, washing and freeze-drying the reaction solution after the heating reaction is finished;
and 3) after the heating reaction is finished, filtering, washing and freeze-drying the reaction liquid.
4. The preparation method of the anode material according to claim 3, wherein the washing step in step 2) is carried out by sequentially washing with N, N-dimethylformamide, ethanol and water, wherein the freeze-drying temperature is-30 ℃ to-40 ℃, and the freeze-drying time is 24 to 48 hours;
and in the step 3), the washing step adopts deionized water for washing, the freeze-drying temperature is-30 ℃ to-40 ℃, and the freeze-drying time is 24-48 h.
5. The method for preparing the anode material according to claim 1 or 2, wherein the step 1) further comprises the steps of filtering, washing and drying the reaction solution after the heating reaction is finished.
6. The preparation method of the anode material according to claim 5, wherein the washing step in the step 1) is carried out by sequentially washing with N, N-dimethylformamide, diethyl ether and methanol, wherein the drying temperature is 80-100 ℃ and the drying time is 24-48 h.
7. The method for producing the anode material according to any one of claims 1 to 6, wherein the heating reaction in step 1) is performed under protection of nitrogen or an inert gas; further comprising the step of purifying the ligand product.
8. The method for producing the anode material according to any one of claims 1 to 7, wherein the first solvent and the second solvent are both N, N-dimethylformamide, and the third solvent is water;
the metal salt is metal nitrate and is selected from at least one of copper nitrate, nickel nitrate and cobalt nitrate.
9. A negative electrode sheet, comprising a current collector and a negative electrode material on the current collector, wherein the negative electrode material is prepared by the preparation method of any one of claims 1 to 8.
10. A lithium ion battery comprising a positive electrode sheet and a negative electrode sheet, wherein the negative electrode sheet is the negative electrode sheet according to claim 9.
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