CN114477130A - Method for preparing hard carbon negative electrode material for sodium ion battery by adopting porous material - Google Patents
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Abstract
The invention discloses a method for preparing a hard carbon negative electrode material for a sodium ion battery by adopting a porous material, which comprises the following steps: the preparation method comprises the steps of coarsely crushing the biomass material cork to obtain cork powder, filtering, drying and screening the cork powder after hydrochloric acid pickling to obtain a porous material, adding the porous material and asphalt into a stirring tank in proportion, stirring and mixing to obtain a hard carbon negative electrode precursor, then putting the hard carbon negative electrode precursor into a rubber mold for pressing to obtain a pressing block, and finally carbonizing the pressing block at high temperature under a protective atmosphere to obtain the hard carbon negative electrode material. The pore space is adjusted by a method for pressing the porous material, and the asphalt is matched to coat the porous material, so that the specific surface area and the porosity of the prepared hard carbon cathode material are reduced, the processing performance of the hard carbon cathode material is improved, the hard carbon cathode material has excellent electrochemical performance, higher first coulombic efficiency and higher circulation capacity, and meanwhile, the preparation process is simple, the preparation cost is lower, and the preparation method is favorable for popularization in the field of sodium ion batteries.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to a method for preparing a hard carbon negative electrode material for a sodium ion battery by adopting a porous material.
Background
With the rapid development of human society and the consumption of traditional fossil energy, the problems of energy crisis and environmental pollution continue to be aggravated, and therefore, it is important to develop efficient energy conversion methods and clean energy systems. At present, lithium ion batteries have become competitive novel energy systems due to their advantages of high power and energy density, long cycle life, good safety, and the like, and are widely applied to daily lives of smart phones, notebook computers, electric vehicles, and the like. However, since the development of large-scale energy storage devices is urgently needed and the reserves of lithium resources are limited, the development of alternatives to lithium ion batteries is required to meet the needs of future development. Sodium is an element widely distributed in nature and is similar to lithium in physical and chemical properties, and therefore, the feasibility of sodium-ion batteries has attracted extensive attention from researchers.
Although sodium ion batteries using sodium ions as charge carriers have great potential in large-scale energy storage systems, they have made significant progress, but the development of negative electrode materials for sodium ion batteries is relatively weak. The negative electrode materials currently studied more are: carbon materials, alloy materials, metal oxides, organic materials, and the like. In the existing method, most of the hard carbon is prepared from a biomass porous material and used as a negative electrode, but the preparation process is complex, the specific surface area and the porosity of the obtained hard carbon negative electrode material are too large, the processing performance is poor, simultaneously, the first coulombic efficiency is low, the circulating capacity is low, and the application to a sodium ion battery is difficult. Therefore, there is a need for an improvement in the existing methods for preparing hard carbon anode materials.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing a hard carbon negative electrode material for a sodium ion battery by using a porous material, which is simple in preparation process, and the prepared hard carbon negative electrode material has a small specific surface area and porosity, so that the hard carbon negative electrode material has good processability, excellent electrochemical performance, high first coulombic efficiency and high cycle capacity.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a hard carbon negative electrode material for a sodium ion battery by adopting a porous material comprises the following steps:
(1) acid washing: coarsely crushing the biomass material cork to obtain cork powder, then pickling the cork powder with hydrochloric acid, filtering, drying and sieving to obtain a porous material;
(2) mixing materials: adding the porous material and the asphalt obtained in the step (1) into a stirring tank according to a proportion, stirring and mixing for 10-30min to obtain a hard carbon cathode precursor;
(3) pressing: putting the hard carbon negative electrode precursor obtained in the step (2) into a rubber mold, and putting the rubber mold into an isostatic pressing forming machine for pressing, wherein the pressure is 80-200MPa, and the pressure maintaining time is 10-30min, so as to obtain a pressing block;
(4) carbonizing: and (4) carbonizing the pressing block obtained in the step (3) at high temperature in a protective atmosphere to obtain the hard carbon negative electrode material.
As a preferred scheme, the biomass material cork is one or more of a wine bottle stopper, a badminton ball support, a bulletin board and a wallboard.
As a preferable scheme, the coarse crushing mode in the step (1) is to perform coarse crushing on the biomass material cork by using one of a crusher, a pulverizer and a wall breaking machine.
Preferably, the drying method in step (1) is drying the washed cork powder by one of sunlight, forced air drying oven and dryer.
As a preferable scheme, the mesh number of the screen used for sieving in the step (1) is 150-400 meshes.
As a preferable mode, D50 of cork powder in the step (1) is 15-30 μm.
As a preferable scheme, the concentration of hydrochloric acid in the step (1) is less than or equal to 12 mol/L.
Preferably, the asphalt is coal-series asphalt or oil-series asphalt, the D50 is 2-10 μm, and the ratio of the porous material to the asphalt is 100: (5-20).
As a preferable mode, the stirring speed in the step (2) is 100-800 rpm.
As a preferable scheme, in the step (4), the temperature is raised to 600 ℃ at a heating rate of 15-25 ℃/min and is kept for 1-3 hours, then the temperature is raised to 1000 ℃ at a heating rate of 10-20 ℃/min and is kept for 4-12 hours, and the hard carbon negative electrode material is obtained after crushing and screening; the protective atmosphere is nitrogen or helium.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and specifically, the technical scheme includes that:
the pore space is adjusted by a method for pressing the porous material, and the asphalt is matched to coat the porous material, so that the specific surface area and the porosity of the prepared hard carbon cathode material are reduced, the processing performance of the hard carbon cathode material is improved, the hard carbon cathode material has excellent electrochemical performance, higher first coulombic efficiency and higher circulation capacity, and meanwhile, the preparation process is simple, the preparation cost is lower, and the preparation method is favorable for popularization in the field of sodium ion batteries.
To more clearly illustrate the features and effects of the present invention, the present invention is described in detail below with reference to specific examples.
Detailed Description
The invention discloses a method for preparing a hard carbon negative electrode material for a sodium ion battery by adopting a porous material, which comprises the following steps:
(1) acid washing: coarsely crushing the biomass material cork to obtain cork powder, then pickling the cork powder with hydrochloric acid, filtering, drying and sieving to obtain a porous material; the biomass cork is one or more of a wine bottle stopper, a badminton support, a bulletin board and a wallboard; the coarse crushing mode of the steps is to perform coarse crushing on the biomass material cork by utilizing one of a crusher, a grinder and a wall breaking machine; the drying mode is to dry the cork powder after acid washing in one mode of sunshine, a blast drying box and a dryer; the mesh number of the screen used for sieving is 150-400 meshes, the D50 of the cork powder is 15-30 mu m, and the hydrochloric acid concentration is less than or equal to 12 mol/L.
(2) Mixing materials: adding the porous material and the asphalt obtained in the step (1) into a stirring tank according to a proportion, stirring and mixing for 10-30min to obtain a hard carbon cathode precursor; the asphalt is coal-series asphalt or oil-series asphalt, the D50 is 2-10 mu m, and the ratio of the porous material to the asphalt is 100: (5-20); the stirring speed is 100-800 rpm;
(3) pressing: putting the hard carbon negative electrode precursor obtained in the step (2) into a rubber mold, and putting the rubber mold into an isostatic pressing forming machine for pressing, wherein the pressure is 80-200MPa, and the pressure maintaining time is 10-30min, so as to obtain a pressing block;
(4) carbonizing: carbonizing the pressing block obtained in the step (3) at high temperature in a protective atmosphere to obtain a hard carbon negative electrode material; specifically, the temperature is raised to 600 ℃ at the temperature raising rate of 15-25 ℃/min and is kept for 1-3 hours, then the temperature is raised to 1000 ℃ at the temperature raising rate of 10-20 ℃/min and is kept for 4-12 hours, and the hard carbon cathode material is obtained after crushing and screening; in addition, the protective atmosphere is nitrogen or helium.
The invention is illustrated in more detail below in the following examples:
example 1
(1) Acid washing: coarsely crushing the biomass material cork to obtain cork powder, then pickling the cork powder with hydrochloric acid, filtering, drying and sieving to obtain a porous material; the biomass cork is a wine bottle stopper; the coarse crushing mode of the step is to perform coarse crushing on the biomass material cork by using a crusher; the drying mode is that the washed cork powder is dried by sunshine; the mesh number of the screen used for sieving is 150 meshes, the D50 of the cork powder is 15-30 μm, and the hydrochloric acid concentration is less than or equal to 12 mol/L.
(2) Mixing materials: adding the porous material and the asphalt obtained in the step (1) into a stirring tank in proportion, and stirring and mixing for 20min to obtain a hard carbon cathode precursor; the asphalt is coal-series asphalt, the D50 is 2-10 mu m, the ratio of the porous material to the asphalt is 100: 10; the stirring speed is 200 rpm;
(3) pressing: putting the hard carbon negative electrode precursor obtained in the step (2) into a rubber mold, and putting the rubber mold into an isostatic pressing forming machine for pressing, wherein the pressure is 100MPa, and the pressure maintaining time is 15min, so as to obtain a pressing block;
(4) carbonizing: carbonizing the pressing block obtained in the step (3) at high temperature in a protective atmosphere to obtain a hard carbon negative electrode material; specifically, heating to 350 ℃ at a heating rate of 18 ℃/min, preserving heat for 2 hours, heating to 800 ℃ at a heating rate of 12 ℃/min, preserving heat for 6 hours, crushing and screening to obtain a hard carbon negative electrode material; in addition, the protective atmosphere is nitrogen.
Example 2
(1) Acid washing: coarsely crushing the biomass material cork to obtain cork powder, then pickling the cork powder with hydrochloric acid, filtering, drying and sieving to obtain a porous material; the biomass material cork is a badminton support; the coarse crushing mode of the step is to perform coarse crushing on the biomass material cork by using a crusher; the drying mode is to dry the washed cork powder through a forced air drying box; the mesh number of the screen used for sieving is 400 meshes, the D50 of the cork powder is 15-30 μm, and the hydrochloric acid concentration is less than or equal to 12 mol/L.
(2) Mixing materials: adding the porous material and the asphalt obtained in the step (1) into a stirring tank in proportion, and stirring and mixing for 15min to obtain a hard carbon cathode precursor; the asphalt is oil asphalt, the D50 is 2-10 μm, the ratio of the porous material to the asphalt is 100: 13; the stirring speed is 500 rpm;
(3) pressing: putting the hard carbon negative electrode precursor obtained in the step (2) into a rubber mold, and putting the rubber mold into an isostatic pressing forming machine for pressing, wherein the pressure is 120MPa, and the pressure maintaining time is 18min, so as to obtain a pressing block;
(4) carbonizing: carbonizing the pressing block obtained in the step (3) at high temperature in a protective atmosphere to obtain a hard carbon negative electrode material; specifically, heating to 400 ℃ at a heating rate of 20 ℃/min, preserving heat for 2 hours, heating to 900 ℃ at a heating rate of 17 ℃/min, preserving heat for 10 hours, crushing and screening to obtain a hard carbon negative electrode material; in addition, the protective atmosphere is helium.
Example 3
(1) Acid washing: coarsely crushing the biomass material cork to obtain cork powder, then pickling the cork powder with hydrochloric acid, filtering, drying and sieving to obtain a porous material; the biomass material cork is a bulletin board; the coarse crushing mode of the steps is to perform coarse crushing on the biomass material cork by using a wall breaking machine; the drying mode is to dry the washed cork powder by a dryer; the mesh number of the screen used for sieving is 200 meshes, the D50 of the cork powder is 15-30 μm, and the hydrochloric acid concentration is less than or equal to 12 mol/L.
(2) Mixing materials: adding the porous material and the asphalt obtained in the step (1) into a stirring tank in proportion, and stirring and mixing for 10min to obtain a hard carbon cathode precursor; the asphalt is coal-series asphalt, the D50 is 2-10 mu m, the ratio of the porous material to the asphalt is 100: 5; the stirring speed is 100 rpm;
(3) pressing: putting the hard carbon negative electrode precursor obtained in the step (2) into a rubber mold, and putting the rubber mold into an isostatic pressing forming machine for pressing, wherein the pressure is 80MPa, and the pressure maintaining time is 10min, so as to obtain a pressing block;
(4) carbonizing: carbonizing the pressing block obtained in the step (3) at high temperature in a protective atmosphere to obtain a hard carbon negative electrode material; specifically, heating to 550 ℃ at a heating rate of 20 ℃/min and preserving heat for 2.5 hours, heating to 680 ℃ at a heating rate of 14 ℃/min and preserving heat for 5 hours, and crushing and screening to obtain a hard carbon negative electrode material; in addition, the protective atmosphere is helium.
Example 4
(1) Acid washing: coarsely crushing the biomass material cork to obtain cork powder, then pickling the cork powder with hydrochloric acid, filtering, drying and sieving to obtain a porous material; the biomass material cork is a wallboard; the coarse crushing mode of the step is to perform coarse crushing on the biomass material cork by using a crusher; the drying mode is that the washed cork powder is dried by sunshine; the mesh number of the screen used for sieving is 250 meshes, the D50 of the cork powder is 15-30 μm, and the hydrochloric acid concentration is less than or equal to 12 mol/L.
(2) Mixing materials: adding the porous material and the asphalt obtained in the step (1) into a stirring tank in proportion, and stirring and mixing for 30min to obtain a hard carbon cathode precursor; the asphalt is coal-series asphalt, the D50 is 2-10 mu m, the ratio of the porous material to the asphalt is 100: 20; the stirring speed is 800 rpm;
(3) pressing: putting the hard carbon negative electrode precursor obtained in the step (2) into a rubber mold, and putting the rubber mold into an isostatic pressing forming machine for pressing, wherein the pressure is 200MPa, and the pressure maintaining time is 30min, so as to obtain a pressing block;
(4) carbonizing: carbonizing the pressing block obtained in the step (3) at high temperature in a protective atmosphere to obtain a hard carbon negative electrode material; specifically, heating to 360 ℃ at a heating rate of 18 ℃/min, preserving heat for 1.5 hours, heating to 700 ℃ at a heating rate of 18 ℃/min, preserving heat for 8 hours, crushing and screening to obtain a hard carbon negative electrode material; in addition, the protective atmosphere is nitrogen.
Example 5
(1) Acid washing: coarsely crushing the biomass material cork to obtain cork powder, then pickling the cork powder with hydrochloric acid, filtering, drying and sieving to obtain a porous material; the biomass material cork is a wallboard; the coarse crushing mode of the steps is to perform coarse crushing on the biomass material cork by using a wall breaking machine; the drying mode is to dry the washed cork powder by a dryer; the mesh number of the screen used for sieving is 350 meshes, the D50 of the cork powder is 15-30 mu m, and the hydrochloric acid concentration is less than or equal to 12 mol/L.
(2) Mixing materials: adding the porous material and the asphalt obtained in the step (1) into a stirring tank in proportion, stirring and mixing for 23min to obtain a hard carbon cathode precursor; the asphalt is oil asphalt, the D50 is 2-10 μm, the ratio of the porous material to the asphalt is 100: 14; the stirring speed is 300 rpm;
(3) pressing: putting the hard carbon negative electrode precursor obtained in the step (2) into a rubber mold, and putting the rubber mold into an isostatic pressing forming machine for pressing, wherein the pressure is 120MPa, and the pressure maintaining time is 20min, so as to obtain a pressing block;
(4) carbonizing: carbonizing the pressing block obtained in the step (3) at high temperature in a protective atmosphere to obtain a hard carbon negative electrode material; specifically, heating to 300 ℃ at a heating rate of 15 ℃/min and preserving heat for 1 hour, heating to 600 ℃ at a heating rate of 10 ℃/min and preserving heat for 4 hours, crushing and screening to obtain a hard carbon negative electrode material; in addition, the protective atmosphere is helium.
Example 6
(1) Acid washing: coarsely crushing the biomass material cork to obtain cork powder, then pickling the cork powder with hydrochloric acid, filtering, drying and sieving to obtain a porous material; the biomass material cork is a wallboard; the coarse crushing mode of the step is to perform coarse crushing on the biomass material cork by using a crusher; the drying mode is that the washed cork powder is dried by sunshine; the mesh number of the screen used for sieving is 250 meshes, the D50 of the cork powder is 15-30 μm, and the hydrochloric acid concentration is less than or equal to 12 mol/L.
2) Mixing materials: adding the porous material and the asphalt obtained in the step (1) into a stirring tank in proportion, and stirring and mixing for 10min to obtain a hard carbon cathode precursor; the asphalt is coal-series asphalt, the D50 is 2-10 mu m, the ratio of the porous material to the asphalt is 100: 5; the stirring speed is 100 rpm;
(3) pressing: putting the hard carbon negative electrode precursor obtained in the step (2) into a rubber mold, and putting the rubber mold into an isostatic pressing forming machine for pressing, wherein the pressure is 80MPa, and the pressure maintaining time is 10min, so as to obtain a pressing block;
(4) carbonizing: carbonizing the pressing block obtained in the step (3) at high temperature in a protective atmosphere to obtain a hard carbon negative electrode material; specifically, the temperature is raised to 600 ℃ at the heating rate of 25 ℃/min and is kept for 3 hours, then the temperature is raised to 600-1000 ℃ at the heating rate of 20 ℃/min and is kept for 12 hours, and the hard carbon negative electrode material is obtained after crushing and screening; in addition, the protective atmosphere is helium.
The hard carbon negative electrode materials prepared in the above embodiments were subjected to performance tests, the test standards are as follows:
particle size distribution: testing according to the method of GB/T19077.1-2016;
moisture content: testing is carried out according to the method of GB/T3521-;
ash content: testing according to the method of GB/T3521-;
specific surface area: testing according to the method of GB/T79587-2017;
first discharge capacity: testing according to the method of GB/T243354-2019;
the first efficiency is as follows: testing according to the method of GB/T243354-2019;
the results of the above tests are shown in tables 1 and 2 below:
TABLE 1
TABLE 2
As can be seen from tables 1 and 2, the hard carbon negative electrode material prepared in the above examples has a smaller specific surface area and a smaller porosity, and the processability of the hard carbon negative electrode material is improved, so that the hard carbon negative electrode material has excellent electrochemical properties, a higher first coulombic efficiency, and a higher cycle capacity.
The design of the invention is characterized in that: the pore space is adjusted by a method for pressing the porous material, and the asphalt is matched to coat the porous material, so that the specific surface area and the porosity of the prepared hard carbon cathode material are reduced, the processing performance of the hard carbon cathode material is improved, the hard carbon cathode material has excellent electrochemical performance, higher first coulombic efficiency and higher circulation capacity, and meanwhile, the preparation process is simple, the preparation cost is lower, and the preparation method is favorable for popularization in the field of sodium ion batteries.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so that any minor modifications, equivalent changes and modifications made to the above embodiment according to the technical spirit of the present invention are within the technical scope of the present invention.
Claims (10)
1. A method for preparing a hard carbon negative electrode material for a sodium ion battery by adopting a porous material is characterized by comprising the following steps: the method comprises the following steps:
(1) acid washing: coarsely crushing the biomass material cork to obtain cork powder, then pickling the cork powder with hydrochloric acid, filtering, drying and sieving to obtain a porous material;
(2) mixing materials: adding the porous material and the asphalt obtained in the step (1) into a stirring tank according to a proportion, stirring and mixing for 10-30min to obtain a hard carbon cathode precursor;
(3) pressing: putting the hard carbon negative electrode precursor obtained in the step (2) into a rubber mold, and putting the rubber mold into an isostatic pressing forming machine for pressing, wherein the pressure is 80-200MPa, and the pressure maintaining time is 10-30min, so as to obtain a pressing block;
(4) carbonizing: and (4) carbonizing the pressing block obtained in the step (3) at high temperature in a protective atmosphere to obtain the hard carbon negative electrode material.
2. The method for preparing the hard carbon anode material for the sodium-ion battery by adopting the porous material as claimed in claim 1, wherein the method comprises the following steps: the biomass material cork is one or more than one of a wine bottle stopper, a badminton support, a bulletin board and a wallboard.
3. The method for preparing the hard carbon anode material for the sodium-ion battery by adopting the porous material as claimed in claim 1, wherein the method comprises the following steps: the coarse crushing mode in the step (1) is to perform coarse crushing on the biomass material cork by utilizing one of a crusher, a pulverizer and a wall breaking machine.
4. The method for preparing the hard carbon anode material for the sodium-ion battery by adopting the porous material as claimed in claim 1, wherein the method comprises the following steps: and (2) drying the washed cork powder in one of a sunshine mode, a forced air drying box and a drying machine in the drying mode in the step (1).
5. The method for preparing the hard carbon anode material for the sodium-ion battery by adopting the porous material according to claim 1, wherein the method comprises the following steps: the mesh number of the screen used for sieving in the step (1) is 150-400 meshes.
6. The method for preparing the hard carbon anode material for the sodium-ion battery by adopting the porous material as claimed in claim 1, wherein the method comprises the following steps: d50=15-30 μm for cork flour in step (1).
7. The method for preparing the hard carbon anode material for the sodium-ion battery by adopting the porous material as claimed in claim 1, wherein the method comprises the following steps: the concentration of hydrochloric acid in the step (1) is less than or equal to 12 mol/L.
8. The method for preparing the hard carbon anode material for the sodium-ion battery by adopting the porous material according to claim 1, wherein the method comprises the following steps: the asphalt is coal-series asphalt or oil-series asphalt, D50=2-10 μm, and the ratio of the porous material to the asphalt is 100: (5-20).
9. The method for preparing the hard carbon anode material for the sodium-ion battery by adopting the porous material as claimed in claim 1, wherein the method comprises the following steps: the stirring speed in the step (2) is 100-800 rpm.
10. The method for preparing the hard carbon anode material for the sodium-ion battery by adopting the porous material according to claim 1, wherein the method comprises the following steps: in the step (4), the temperature is raised to 600 ℃ of 300-; the protective atmosphere is nitrogen or helium.
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| CN115304052A (en) * | 2022-10-13 | 2022-11-08 | 溧阳天目先导电池材料科技有限公司 | Wood-based composite hard carbon negative electrode material and preparation method and application thereof |
| CN115744871A (en) * | 2022-11-26 | 2023-03-07 | 中南大学 | Bagasse-based sodium ion battery hard carbon negative electrode active material, and preparation and application thereof |
| CN115991465A (en) * | 2022-11-22 | 2023-04-21 | 昆明理工大学 | Hard carbon material applied to sodium ion battery and preparation method thereof |
| CN116040610A (en) * | 2023-02-20 | 2023-05-02 | 兰州宏彬新能源发展有限公司 | Preparation method of porous biomass hard carbon composite material |
| CN116062731A (en) * | 2023-02-07 | 2023-05-05 | 湖北万润新能源科技股份有限公司 | Method for preparing hard carbon |
| CN117466284A (en) * | 2023-12-28 | 2024-01-30 | 天津理工大学 | Surface modified hard carbon negative electrode material of sodium ion battery and preparation method thereof |
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| CN115304052A (en) * | 2022-10-13 | 2022-11-08 | 溧阳天目先导电池材料科技有限公司 | Wood-based composite hard carbon negative electrode material and preparation method and application thereof |
| CN115991465A (en) * | 2022-11-22 | 2023-04-21 | 昆明理工大学 | Hard carbon material applied to sodium ion battery and preparation method thereof |
| CN115991465B (en) * | 2022-11-22 | 2023-09-26 | 昆明理工大学 | Hard carbon material applied to sodium ion battery and preparation method thereof |
| CN115744871A (en) * | 2022-11-26 | 2023-03-07 | 中南大学 | Bagasse-based sodium ion battery hard carbon negative electrode active material, and preparation and application thereof |
| CN116062731A (en) * | 2023-02-07 | 2023-05-05 | 湖北万润新能源科技股份有限公司 | Method for preparing hard carbon |
| CN116040610A (en) * | 2023-02-20 | 2023-05-02 | 兰州宏彬新能源发展有限公司 | Preparation method of porous biomass hard carbon composite material |
| CN117466284A (en) * | 2023-12-28 | 2024-01-30 | 天津理工大学 | Surface modified hard carbon negative electrode material of sodium ion battery and preparation method thereof |
| CN117466284B (en) * | 2023-12-28 | 2024-03-15 | 天津理工大学 | Surface modified hard carbon negative electrode material of sodium ion battery and preparation method thereof |
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