CN111498842A - Preparation method of ferrous sulfide asphalt-based composite spherical activated carbon - Google Patents
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- C01B32/30—Active carbon
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- 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
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Abstract
The invention relates to a preparation method of ferrous sulfide asphalt-based composite spherical activated carbon, which comprises the steps of carrying out Soxhlet extraction on coal tar medium-temperature asphalt by taking pyridine as a solvent, wherein the extraction time is 4-5 hours, cooling an extraction solution, carrying out suction filtration and collecting filtrate; mixing polyvinyl alcohol, absolute ethyl alcohol and deionized water, heating the mixture in a water bath until the polyvinyl alcohol is completely dissolved, cooling the mixture to room temperature, adding ferrous sulfide powder, and performing ultrasonic treatment; heating, stirring at constant temperature and cooling to room temperature; under the condition of air, the temperature is raised to 300 ℃, and the temperature is cooled, and the temperature is raised to 680-700 ℃ under the nitrogen atmosphere, and the temperature is cooled. The advantages are that: the finished product of the active carbon cathode material has good cycle performance, and solves the problems of volume expansion, poor conductivity and the like of the ferrous sulfide electrode material in the cycle process.
Description
Technical Field
The invention belongs to a negative electrode material of a lithium ion battery, and relates to a preparation method of ferrous sulfide asphalt-based composite spherical activated carbon.
Background
The coal pitch is the residue of coal tar after distilling and extracting liquid fraction, accounts for about 50-60% of the total amount of the coal tar, is an important coking byproduct, has the characteristics of high aromaticity, high carbon content, low metal impurity content and the like, and is an excellent precursor for preparing carbon materials.
The asphalt-based spherical activated carbon has the advantages of large specific surface area, good mechanical property, excellent adsorption property, uniform filling density, rich pore structure and the like, and is widely applied to the aspects of electrode materials, catalysts, environmental protection and the like.
The sulfur element and the iron element are rich elements on the earth, the raw materials of the two elements are low in price, and the compound ferrous sulfide formed by the two elements is greatly concerned as a lithium storage material in recent years++2e-→Fe+Li2S, corresponding to a platform of 1.6V in a charge-discharge curve, the theoretical specific capacity is 609mAhg-1About 4 times of the lithium cobaltate positive electrode material. The material has the advantages of high energy density, low toxicity and the like as an electrode material of a lithium ion battery, and becomes one of potential choices of the electrode material of the next generation lithium ion battery. However, due to the low electronic conductivity and the huge volume change in the lithium storage process, the electrode material is pulverized, so that the electrode has poor cycle performance and poor rate capability, and the coal tar pitch carbon can be selected to coat the electrode material to solve the problems.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of ferrous sulfide asphalt-based composite spherical activated carbon, which can inhibit the problems of poor charge-discharge cycle performance, small discharge specific capacity and low conductivity of ferrous sulfide as a lithium ion battery cathode material.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of ferrous sulfide asphalt-based composite spherical activated carbon comprises the following steps:
1) performing Soxhlet extraction on coal tar medium temperature pitch by taking pyridine as a solvent, performing Soxhlet extraction on 80-150ml of pyridine and 0.5-1.5g of coal tar medium temperature pitch for 4-5 hours, cooling an extraction solution, performing suction filtration and collecting filtrate;
2) mixing 1788 type polyvinyl alcohol, absolute ethyl alcohol and deionized water according to the mass ratio of 2.25: 21.33: 150, heating to 90-95 ℃ in a water bath kettle to ensure that the polyvinyl alcohol is completely dissolved, and finally cooling to room temperature;
3) mixing the solutions obtained in the steps 1) and 2), adding 0.1-0.3g of ferrous sulfide powder, and performing ultrasonic treatment for 2-5 min;
4) heating the mixed solution after ultrasonic treatment to 83-85 ℃, and then stirring at constant temperature for 15-20 min;
5) cooling the stirred solution to room temperature, and performing suction filtration to obtain a ferrous sulfide asphalt-based composite spherical activated carbon precursor;
6) heating the ferrous sulfide asphalt-based composite spherical activated carbon precursor from room temperature to 300 ℃ under the air condition, wherein the heating rate is 0.10-0.15 ℃/min, keeping the temperature at 300 ℃ for 3-4 hours, and taking out a sample after natural cooling; the sample is heated from room temperature to 680-700 ℃ under the nitrogen atmosphere, the heating rate is 2.75-2.85 ℃/min, the temperature is kept constant at 680-700 ℃ for 3-4 hours, and the sample is taken out after natural cooling to obtain a finished product, namely the ferrous sulfide asphalt-based composite spherical activated carbon.
The density of the absolute ethyl alcohol is 0.79 g/ml.
The medium temperature pitch of the coal tar is below 100 meshes.
Compared with the prior art, the invention has the beneficial effects that:
the ferrous sulfide asphalt-based composite spherical activated carbon cathode material prepared by the method has good cycle performance, and solves the problems of volume expansion, poor conductivity and the like of the ferrous sulfide electrode material in the cycle process. After the ferrous sulfide asphalt-based composite spherical activated carbon doped with 0.1g, 0.2g and 0.3g is circulated for 40 circles, the discharge capacities are respectively 194.5mAh/g, 175.8mAh/g and 169.5mAh/g, and the coulombic efficiency is close to 100 percent.
Drawings
FIG. 1 is a flow chart of a production process of ferrous sulfide asphalt-based composite spherical activated carbon.
FIG. 2 is an XRD diagram of ferrous sulfide asphalt-based composite spherical activated carbon.
In fig. 2: a is the XRD curve of the composite asphalt ball doped with 0.1 gFeS; b is the XRD curve of the composite asphalt ball doped with 0.2g of FeS; and c is the XRD curve of the composite asphalt ball doped with 0.3g of FeS.
FIG. 3 is a scanning electron micrograph of FeS-doped composite asphalt spheres.
In fig. 3: (a) and (b) is a scanning electron microscope picture and a partial enlarged view of the composite asphalt ball doped with 0.1g of FeS; (c) and (d) a scanning electron microscope image and a partial enlarged view of the composite asphalt ball doped with 0.2g of FeS; (e) and (f) is a scanning electron microscope image and a partial enlarged view of the composite asphalt ball doped with 0.3g of FeS.
FIG. 4 is a graph of electrochemical performance of FeS-doped composite asphalt spheres.
In fig. 4: (a) and (b) is a multiplying power performance and cycle performance diagram of the composite asphalt ball doped with 0.1 gFeS; (c) and (d) is a multiplying power performance and cycle performance diagram of the composite asphalt ball doped with 0.2g of FeS; (e) and (f) is a multiplying power performance and cycle performance diagram of the composite asphalt ball doped with 0.3g of FeS.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings, but it should be noted that the present invention is not limited to the following embodiments.
Example 1
Referring to fig. 1, a preparation method of ferrous sulfide asphalt-based composite spherical activated carbon comprises the following steps:
1) performing Soxhlet extraction on 0.5-1.5g of coal tar medium temperature pitch (the particle size is 100 meshes) by taking 80-150ml of pyridine as a solvent for 4-5 hours, cooling the extraction solution, performing suction filtration and collecting filtrate; preferably, 80, 100, 120, 150ml of pyridine and 0.5, 1, 1.2 and 1.5g of coal tar medium temperature pitch are taken for Soxhlet extraction;
2) mixing 2.25g of polyvinyl alcohol 1788 type, 27ml of absolute ethanol (density 0.79g/ml) and 150ml of deionized water, heating to 90-95 ℃, preferably 90 ℃, 92 ℃ and 95 ℃ in a water bath kettle to ensure that the polyvinyl alcohol is completely dissolved, and finally cooling to room temperature;
3) mixing the solutions obtained in step 1) and step 2), adding ferrous sulfide powder 0.1-0.3g, and performing ultrasonic treatment for 2-5min, preferably 2, 3, 4, 5 min;
4) heating the mixed solution after ultrasonic treatment to 83-85 deg.C, preferably 83, 85, 84 deg.C, and stirring at constant temperature for 15-20min, preferably 15, 18, 20 min;
5) cooling the stirred solution to room temperature, and performing suction filtration to obtain a ferrous sulfide asphalt-based composite spherical activated carbon precursor;
6) heating the ferrous sulfide asphalt-based composite spherical activated carbon precursor from room temperature to 300 ℃ under the air condition, wherein the heating rate is 0.1-0.15 ℃/min, preferably 0.1, 0.12, 0.13 and 0.15 ℃/min, keeping the temperature at 300 ℃ for 3-4 hours, preferably 4 hours, and taking out a sample after natural cooling; the sample is heated from room temperature to 680-700 ℃ in the nitrogen atmosphere, preferably 680, 685, 688 and 700 ℃, the heating rate is 2.75-2.85 ℃/min, preferably 2.75, 2.78, 2.81 and 2.85 ℃/min, the sample is kept at the constant temperature of 700 ℃ for 3-4 hours, preferably 4 hours, and the sample is taken out after natural cooling, so that the finished product, namely the ferrous sulfide asphalt base composite spherical activated carbon, is obtained.
The assembly process of the lithium ion battery comprises the preparation of electrode plates and the assembly process of the lithium ion battery, and specifically comprises the following steps:
1. weighing ferrous sulfide asphalt-based composite spherical activated carbon, a conductive agent (Super-P) and a binder (PVDF) according to a mass ratio of 8:1:1, grinding and mixing uniformly, adding N-methyl pyrrolidone (NMP) to mix into viscous slurry, and then coating the slurry on the surface of a current collector (copper foil) uniformly by using a film coater.
2. And (3) putting the copper foil coated with the slurry into a vacuum oven at 120 ℃ for baking for 12h, and removing the NMP solvent. And finally, cutting the copper foil into circular electrode plates with the diameter of 11mm for later use. The sequence of packaging the batteries is as follows: negative electrode shell, lithium piece, diaphragm, negative electrode piece, gasket, spring leaf, positive electrode shell. The lithium sheet served as the counter and reference electrodes throughout the test element. The whole process of packaging the lithium ion battery is carried out in a glove box filled with argon, and the water and oxygen content is less than 0.1 ppm.
FIG. 2 is an XRD pattern of the sample obtained in example 1, and a, b and c are curves doped with 0.1g, 0.2 and 0.3g of FeS, respectively. As can be seen from the figure, the curves in the obtained samples all correspond to the standard peak of FeS of the standard card, which indicates that the ferrous sulfide asphalt-based composite material is successfully prepared.
Fig. 3 is an SEM picture of the sample obtained in example 1, and it can be seen from fig. 3 that the prepared sample is spherical and has good sphericity, and the XRD curve shows that the ferrous sulfide pitch-based composite spherical activated carbon is successfully prepared.
Fig. 4(a) and (b) are graphs of the rate and cycle performance of example 1 doping with 0.1g fes. As can be seen from FIG. 4(a), the specific discharge capacity after 10 cycles at a current density of 100mA/g was 223.9mAh/g, and then the current densities were adjusted to 200, 500, 1000, 2000 and 5000mA/g, and the discharge capacities after 10 cycles were 230.8, 194.4, 140.0, 74.4 and 25mAh/g, respectively. Finally, the current density is regulated back to 100mAh/g, and the discharge specific capacity of the sample still returns to 245.8mAh/g after 10 cycles of circulation, which shows that the sample structure is not greatly influenced after high-current charge and discharge and shows good rate performance; as can be seen from fig. 4(b), the capacity of the sample gradually decreases during the cycling process, the specific discharge capacity of the first turn of the sample is 509.9mAh/g, and the coulombic efficiency is 53.75%. After 2 and 3 cycles, the coulombic efficiency rapidly increased to 94.56%. After 17 cycles the capacity dropped to 198.6mAh/g, the coulombic efficiency was 99.89%, and the capacity remained essentially stable over the following cycles. After 40 cycles, the capacity was 194.5mAh/g, and the coulombic efficiency was 99.84%.
FIGS. 4(c) and (d) are graphs of the multiplying power and the cycle performance of the composite asphalt ball doped with 0.2gFeS in example 1. As can be seen from FIG. 4(c), the specific discharge capacity was 172mAh/g after 10 cycles at a current density of 100mA/g, and then the discharge capacities after 10 cycles were adjusted to 200, 500, 1000, 2000 and 5000mA/g to 136.3, 96.2, 60.3, 33.9 and 12mAh/g, respectively. Finally, the current density is adjusted to 100mAh/g, the discharge specific capacity of the sample still returns to 170.3mAh/g after 10 cycles of circulation, which shows that the large-current charge-discharge has little influence on the sample structure and shows good rate performance; from FIG. 4(d), the capacity of the sample during the circulation process is gradually reduced, the specific discharge capacity of the first circle of the sample is 529mAh/g, and the coulombic efficiency is 71.85%. After 2 and 3 cycles, the coulombic efficiency rapidly increased to 94.72%. After 17 cycles the capacity dropped to 198.7mAh/g, the coulombic efficiency was 98.11%, and the capacity remained essentially stable in the following cycles. After 40 cycles, the capacity is 175.8mAh/g, and the coulombic efficiency is 99.54%.
FIGS. 4(e) and (f) are graphs of the multiplying power and the cycle performance of the composite asphalt ball doped with 0.3gFeS in example 1. As can be seen from FIG. 4(e), the specific discharge capacity of 211.4mAh/g was obtained after 10 cycles at a current density of 100mA/g, and then the discharge capacities after 10 cycles were adjusted to 200, 500, 1000, 2000 and 5000mA/g to 152.9, 112.5, 74.4, 46.7 and 24.8mAh/g, respectively. Finally, the current density is adjusted to return to 100mAh/g again, the discharge specific capacity still returns to 171.4mAh/g after 10 cycles of circulation, which shows that the sample structure is not greatly influenced after the large-current charge and discharge, and the good rate performance is shown; as can be seen from fig. 4(f), the capacity gradually decreases during the circulation process, the specific discharge capacity of the first turn of the sample is 589.5mAh/g, and the coulombic efficiency is 63.79%. After 2 and 3 cycles, the coulombic efficiency rapidly increased to 91.09%. After 17 cycles, the capacity dropped to 189.3mAh/g, the coulombic efficiency was 98.37%, and the capacity remained substantially constant in the following cycles. After 40 cycles, the capacity is 169.5mAh/g, and the coulombic efficiency is 100.1%.
Claims (3)
1. A preparation method of ferrous sulfide asphalt-based composite spherical activated carbon is characterized by comprising the following steps:
1) performing Soxhlet extraction on coal tar medium temperature pitch by taking pyridine as a solvent, performing Soxhlet extraction on 80-150ml of pyridine and 0.5-1.5g of coal tar medium temperature pitch for 4-5 hours, cooling an extraction solution, performing suction filtration and collecting filtrate;
2) mixing 1788 type polyvinyl alcohol, absolute ethyl alcohol and deionized water according to the mass ratio of 2.25: 21.33: 150, heating to 90-95 ℃ in a water bath kettle to ensure that the polyvinyl alcohol is completely dissolved, and finally cooling to room temperature;
3) mixing the solutions obtained in the steps 1) and 2), adding 0.1-0.3g of ferrous sulfide powder, and performing ultrasonic treatment for 2-5 min;
4) heating the mixed solution after ultrasonic treatment to 83-85 ℃, and then stirring at constant temperature for 15-20 min;
5) cooling the stirred solution to room temperature, and performing suction filtration to obtain a ferrous sulfide asphalt-based composite spherical activated carbon precursor;
6) heating the ferrous sulfide asphalt-based composite spherical activated carbon precursor from room temperature to 300 ℃ under the air condition, wherein the heating rate is 0.10-0.15 ℃/min, keeping the temperature at 300 ℃ for 3-4 hours, and taking out a sample after natural cooling; the sample is heated from room temperature to 680-700 ℃ under the nitrogen atmosphere, the heating rate is 2.75-2.85 ℃/min, the temperature is kept constant at 680-700 ℃ for 3-4 hours, and the sample is taken out after natural cooling to obtain a finished product, namely the ferrous sulfide asphalt-based composite spherical activated carbon.
2. The method for preparing ferrous sulfide asphalt-based composite spherical activated carbon according to claim 1, wherein the density of the absolute ethyl alcohol is 0.79 g/ml.
3. The method for preparing ferrous sulfide pitch-based composite spherical activated carbon according to claim 1, wherein the medium temperature pitch of coal tar is 100 mesh below.
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2020
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| WO2014162693A1 (en) * | 2013-04-02 | 2014-10-09 | 出光興産株式会社 | Composite material |
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