CN114188516A - High-rate negative electrode material and preparation method thereof - Google Patents
High-rate negative electrode material and preparation method thereof Download PDFInfo
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- CN114188516A CN114188516A CN202111408764.0A CN202111408764A CN114188516A CN 114188516 A CN114188516 A CN 114188516A CN 202111408764 A CN202111408764 A CN 202111408764A CN 114188516 A CN114188516 A CN 114188516A
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Abstract
The invention discloses a preparation method of a high-rate negative electrode material, which comprises, by weight, 10-50 parts of petroleum coke, 20-100 parts of an oxidizing agent, 20-100 parts of a reducing agent and 1-5 parts of a modifying agent. The petroleum coke carbon is jointly modified by methods such as mechanical ball milling treatment, oxidation-reduction treatment, fluorination modification and the like, so that the first coulombic efficiency, the first circulation capacity, the first circulation frequency and the multiplying power charge and discharge are improved.
Description
Technical Field
The invention relates to the technical field of new energy, in particular to a high-rate negative electrode material and a preparation method thereof.
Background
Petroleum coke is a byproduct of petroleum refining processes and is a black solid or powder produced by delayed coking units. Petroleum coke is classified into needle coke, sponge coke and shot coke according to its structure and appearance. The petroleum coke is used as the negative electrode material of the lithium ion battery, and the electrochemical performance of the petroleum coke is between the hard carbon material and the graphite material. Not only keeps the low voltage platform of graphite material lithium embedding, but also has higher capacity of hard carbon, and is an ideal choice for the cathode material of the lithium ion battery. In addition, petroleum coke materials are rich in resources, low in price, green and pollution-free, and are hot spots for the research of lithium ion negative electrode materials at the present stage.
In the preparation process of the electrode, petroleum coke carbon with the particle size of 49 mu m cannot be well used, the overall quality of the battery is affected, the defect of poor doping effect exists in the preparation process, and the petroleum coke carbon is frequently discarded without use, so that the material waste is caused.
Therefore, we propose a high-rate negative electrode material and a preparation method thereof to solve the above problems.
Disclosure of Invention
The present invention is intended to provide a high-rate anode material and a method for preparing the same to solve the problems set forth in the background art.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-rate negative electrode material comprises, by weight, 10-50 parts of petroleum coke, 20-100 parts of an oxidizing agent, 20-100 parts of a reducing agent and 1-5 parts of a modifying agent.
Preferably, the additive comprises 20 parts of petroleum coke, 40 parts of oxidizing agent, 40 parts of reducing agent and 2 parts of modifying agent by weight.
Preferably, the additive comprises 40 parts by weight of petroleum coke, 80 parts by weight of oxidant, 80 parts by weight of reducing agent and 2 parts by weight of modifier.
The high-rate negative electrode material can be prepared by adopting other raw materials in parts by weight.
The preparation method of the high-rate negative electrode material comprises the following steps:
s1, selecting granular petroleum coke as a petroleum carbon raw material, and crushing the petroleum carbon raw material;
s2, carrying out oxidation reduction treatment on the petroleum coke treated by the S1;
s21, oxidizing the petroleum coke treated by the S1 by using an oxidizing agent;
s22, reducing the petroleum coke treated by the S21 by using a reducing agent;
s3, the petroleum coke after the treatment of S2 is fluorinated and modified.
Untreated petroleum coke has a high capacity of being discharged for the first time, but the capacity of being charged for the first time is less than half of the capacity of being discharged for the first time, the first coulombic efficiency is low and far lower than the material standard, and therefore improvement is made in the aspects of improving the first coulombic efficiency, the capacity of being circulated and the cycle rate performance.
Preferably, the S1 includes the steps of:
s11, mechanically crushing the petroleum carbon raw material by using a planetary ball mill and a ball milling medium, wherein the crushing grain size is within 15 mu m;
the planetary ball mill can be used for pulverizing petroleum coke into a pulverized particle size of 15 μm or less by a high-speed pulverizer, as compared with a mortar mill, and can be used for the shortest time.
S12, in the course of S11, particle size analysis was performed using a laser particle size analyzer or SEM.
Compared with a laser particle size analyzer, SEM can more intuitively observe the change of the carbon structure of petroleum coke, and therefore, the SEM is used as a main analysis means. The petroleum coke carbon material and the graphite material have similar layered structures, and compared with the layered structure of graphite, the petroleum coke has a more disordered structure and good compatibility. The first coulombic efficiency is improved along with the reduction of the particle size of the graphite coke.
Preferably, the ball milling medium in S11 is ethanol, which is more environmentally friendly than other materials.
Preferably, the S21 includes the steps of:
s211, placing 1 part by weight of petroleum coke into a container, adding 2 parts by weight of oxidant to immerse the petroleum coke, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s212, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃.
Preferably, the oxidant is H2O2、HNO3、H2SO4、KMnO4、K2Cr2O7。
The petroleum coke after oxidation treatment has improved circulation capacity and initial coulomb efficiency.
Preferably, the S22 includes the steps of:
s221, putting 1 part by weight of petroleum coke into a container, adding 2 parts by weight of reducing solution, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s222, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃.
The petroleum coke after reduction treatment has slightly improved circulation capacity and first coulombic efficiency.
Preferably, the S3 includes the steps of:
s31, putting the petroleum coke with the mass of 1 into a container, adding water with the mass of 1.5 for dissolving and dispersing, and adding LINO with the mass of 0.08-0.13Magnetically stirring for 2h at the ambient temperature of 20-25 ℃;
s32, adding modifier NH with the mass ratio of 0.04-0.054HF2Performing magnetic stirring for 8 hours, performing suction filtration by using a suction filtration device, placing the mixture in an oven for drying and grinding, wherein the temperature of a drying box is 100 ℃;
and S33, roasting the coated powder for 12 hours under the protection of nitrogen atmosphere, wherein the roasting temperature is 500 ℃, and thus obtaining a coated product.
The coating can make up the problem of capacity reduction after ball milling, the first coulomb efficiency after ball milling is kept, and the modification is more successful.
The high-rate negative electrode material prepared by the method has excellent performances in the aspects of initial coulombic efficiency, cycle times and rate charge and discharge.
Compared with the prior art, the invention has the beneficial effects that:
the petroleum coke carbon is jointly modified by methods such as mechanical ball milling treatment, oxidation-reduction treatment, fluorination modification and the like, so that the first coulombic efficiency, the first circulation capacity, the first circulation frequency and the multiplying power charge and discharge are improved.
Drawings
Fig. 1 is a flow chart of a method for preparing a high-rate negative electrode material according to the present invention;
fig. 2 is a flowchart of a method S1 for preparing a high-rate negative electrode material according to the present invention;
fig. 3 is a flowchart of a method S2 for preparing a high-rate negative electrode material according to the present invention;
fig. 4 is a flowchart of a method S21 for preparing a high-rate negative electrode material according to the present invention;
fig. 5 is a flowchart of a method S22 for preparing a high-rate negative electrode material according to the present invention;
fig. 6 is a flowchart of a method S3 for preparing a high-rate negative electrode material according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
The high-rate negative electrode material comprises, by weight, 10-50 parts of petroleum coke, 20-100 parts of an oxidizing agent, 20-100 parts of a reducing agent and 1-5 parts of a modifying agent.
Specifically, the additive comprises 20 parts by weight of petroleum coke, 40 parts by weight of an oxidizing agent, 40 parts by weight of a reducing agent and 2 parts by weight of a modifying agent.
Example 2
The present embodiment is different from embodiment 1 in that: the composite material comprises, by weight, 40 parts of petroleum coke, 80 parts of an oxidizing agent, 80 parts of a reducing agent and 2 parts of a modifying agent.
Example 3
Referring to fig. 1 to 6, a method for preparing a high-rate negative electrode material, the method comprising the steps of:
s1, selecting granular petroleum coke as a petroleum carbon raw material, and crushing the petroleum carbon raw material;
s1 includes the steps of:
s11, mechanically crushing the petroleum carbon raw material by using a planetary ball mill and a ball milling medium, wherein the crushing grain size is within 15 mu m;
the ball milling medium in S11 is ethanol;
s12, in the S11 process, a laser particle size analyzer or SEM is used for analyzing the particle size;
s2, carrying out oxidation reduction treatment on the petroleum coke treated by the S1;
s21, oxidizing the petroleum coke treated by the S1 by using an oxidizing agent;
the oxidant is H2O2；
S21 includes the steps of:
s211, placing 1 part by weight of petroleum coke into a container, adding 2 parts by weight of oxidant to immerse the petroleum coke, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s212, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s22, reducing the petroleum coke treated by the S21 by using a reducing agent;
s22 includes the steps of:
s221, putting 1 part by weight of petroleum coke into a container, adding 2 parts by weight of reducing solution, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s222, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s3, performing fluorination modification on the petroleum coke after the treatment of S2;
s3 includes the steps of:
s31, putting the petroleum coke with the mass of 1 into a container, adding water with the mass of 1.5 for dissolving and dispersing, and adding LINO with the mass of 0.08-0.13Magnetically stirring for 2h at the ambient temperature of 20-25 ℃;
s32, adding modifier NH with the mass ratio of 0.04-0.054HF2Performing magnetic stirring for 8 hours, performing suction filtration by using a suction filtration device, placing the mixture in an oven for drying and grinding, wherein the temperature of a drying box is 100 ℃;
and S33, roasting the coated powder for 12 hours under the protection of nitrogen atmosphere, wherein the roasting temperature is 500 ℃, and thus obtaining a coated product.
Example 4
Referring to fig. 1 to 6, a method for preparing a high-rate negative electrode material, the method comprising the steps of:
s1, selecting granular petroleum coke as a petroleum carbon raw material, and crushing the petroleum carbon raw material;
s1 includes the steps of:
s11, mechanically crushing the petroleum carbon raw material by using a planetary ball mill and a ball milling medium, wherein the crushing grain size is within 15 mu m;
the ball milling medium in S11 is ethanol;
s12, in the S11 process, a laser particle size analyzer or SEM is used for analyzing the particle size;
s2, carrying out oxidation reduction treatment on the petroleum coke treated by the S1;
s21, oxidizing the petroleum coke treated by the S1 by using an oxidizing agent;
the oxidant is HNO3；
S21 includes the steps of:
s211, placing 1 part by weight of petroleum coke into a container, adding 2 parts by weight of oxidant to immerse the petroleum coke, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s212, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s22, reducing the petroleum coke treated by the S21 by using a reducing agent;
s22 includes the steps of:
s221, putting 1 part by weight of petroleum coke into a container, adding 2 parts by weight of reducing solution, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s222, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s3, performing fluorination modification on the petroleum coke after the treatment of S2;
s3 includes the steps of:
s31, putting the petroleum coke with the mass of 1 into a container, adding water with the mass of 1.5 for dissolving and dispersing, and adding LINO with the mass of 0.08-0.13Magnetically stirring for 2h at the ambient temperature of 20-25 ℃;
s32, adding modifier NH with the mass ratio of 0.04-0.054HF2Performing magnetic stirring for 8 hours, performing suction filtration by using a suction filtration device, placing the mixture in an oven for drying and grinding, wherein the temperature of a drying box is 100 ℃;
and (3) roasting the S33 coated powder for 12h under the protection of nitrogen atmosphere, wherein the roasting temperature is 500 ℃, and thus obtaining a coated product.
Example 5
Referring to fig. 1 to 6, a method for preparing a high-rate negative electrode material, the method comprising the steps of:
s1, selecting granular petroleum coke as a petroleum carbon raw material, and crushing the petroleum carbon raw material;
s1 includes the steps of:
s11, mechanically crushing the petroleum carbon raw material by using a planetary ball mill and a ball milling medium, wherein the crushing grain size is within 15 mu m;
the ball milling medium in S11 is ethanol;
s12, in the S11 process, a laser particle size analyzer or SEM is used for analyzing the particle size;
s2, carrying out oxidation reduction treatment on the petroleum coke treated by the S1;
s21, oxidizing the petroleum coke treated by the S1 by using an oxidizing agent;
the oxidant is H2SO4；
S21 includes the steps of:
s211, placing 1 part by weight of petroleum coke into a container, adding 2 parts by weight of oxidant to immerse the petroleum coke, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s212, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s22, reducing the petroleum coke treated by the S21 by using a reducing agent;
s22 includes the steps of:
s221, putting 1 part by weight of petroleum coke into a container, adding 2 parts by weight of reducing solution, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s222, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s3, performing fluorination modification on the petroleum coke after the treatment of S2;
s3 includes the steps of:
s31, putting the petroleum coke with the mass of 1 into a container, adding water with the mass of 1.5 for dissolving and dispersing, and adding LINO with the mass of 0.08-0.13Magnetically stirring for 2h at the ambient temperature of 20-25 ℃;
s32, adding modifier NH with the mass ratio of 0.04-0.054HF2Performing magnetic stirring for 8 hours, performing suction filtration by using a suction filtration device, placing the mixture in an oven for drying and grinding, wherein the temperature of a drying box is 100 ℃;
and S33, roasting the coated powder for 12 hours under the protection of nitrogen atmosphere, wherein the roasting temperature is 500 ℃, and thus obtaining a coated product.
Example 6
Referring to fig. 1 to 6, a method for preparing a high-rate negative electrode material, the method comprising the steps of:
s1, selecting granular petroleum coke as a petroleum carbon raw material, and crushing the petroleum carbon raw material;
s1 includes the steps of:
s11, mechanically crushing the petroleum carbon raw material by using a planetary ball mill and a ball milling medium, wherein the crushing grain size is within 15 mu m;
the ball milling medium in S11 is ethanol;
s12, in the S11 process, a laser particle size analyzer or SEM is used for analyzing the particle size;
s2, carrying out oxidation reduction treatment on the petroleum coke treated by the S1;
s21, oxidizing the petroleum coke treated by the S1 by using an oxidizing agent;
the oxidant is KMnO4；
S21 includes the steps of:
s211, placing 1 part by weight of petroleum coke into a container, adding 2 parts by weight of oxidant to immerse the petroleum coke, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s212, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s22, reducing the petroleum coke treated by the S21 by using a reducing agent;
s22 includes the steps of:
s221, putting 1 part by weight of petroleum coke into a container, adding 2 parts by weight of reducing solution, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s222, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s3, performing fluorination modification on the petroleum coke after the treatment of S2;
s3 includes the steps of:
s31, putting the petroleum coke with the mass of 1 into a container, adding water with the mass of 1.5 for dissolving and dispersing, and adding LINO with the mass of 0.08-0.13Magnetically stirring for 2h at the ambient temperature of 20-25 ℃;
s32, adding modifier NH with the mass ratio of 0.04-0.054HF2Performing magnetic stirring for 8 hours, performing suction filtration by using a suction filtration device, placing the mixture in an oven for drying and grinding, wherein the temperature of a drying box is 100 ℃;
and (3) roasting the S33 coated powder for 12h under the protection of nitrogen atmosphere, wherein the roasting temperature is 500 ℃, and thus obtaining a coated product.
Example 7
Referring to fig. 1 to 6, a method for preparing a high-rate negative electrode material, the method comprising the steps of:
s1, selecting granular petroleum coke as a petroleum carbon raw material, and crushing the petroleum carbon raw material;
s1 includes the steps of:
s11, mechanically crushing the petroleum carbon raw material by using a planetary ball mill and a ball milling medium, wherein the crushing grain size is within 15 mu m;
the ball milling medium in S11 is ethanol;
s12, in the S11 process, a laser particle size analyzer or SEM is used for analyzing the particle size;
s2, carrying out oxidation reduction treatment on the petroleum coke treated by the S1;
s21, oxidizing the petroleum coke treated by the S1 by using an oxidizing agent;
the oxidant is K2Cr2O7；
S21 includes the steps of:
s211, placing 1 part by weight of petroleum coke into a container, adding 2 parts by weight of oxidant to immerse the petroleum coke, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s212, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s22, reducing the petroleum coke treated by the S21 by using a reducing agent;
s22 includes the steps of:
s221, putting 1 part by weight of petroleum coke into a container, adding 2 parts by weight of reducing solution, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s222, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃;
s3, performing fluorination modification on the petroleum coke after the treatment of S2;
s3 includes the steps of:
s31, placing the petroleum coke with the mass of 1 into a container, adding water with the mass of 1.5 for dissolving and dispersing, and adding the water with the mass of 0.08-0.1 LINO3Magnetically stirring for 2h at the ambient temperature of 20-25 ℃;
s32, adding modifier NH with the mass ratio of 0.04-0.054HF2Performing magnetic stirring for 8 hours, performing suction filtration by using a suction filtration device, placing the mixture in an oven for drying and grinding, wherein the temperature of a drying box is 100 ℃;
and (3) roasting the S33 coated powder for 12h under the protection of nitrogen atmosphere, wherein the roasting temperature is 500 ℃, and thus obtaining a coated product.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The high-rate negative electrode material is characterized in that: the additive comprises, by weight, 10-50 parts of petroleum coke, 20-100 parts of an oxidant, 20-100 parts of a reducing agent and 1-5 parts of a modifier.
2. The high-rate anode material according to claim 1, characterized in that: the composite material comprises, by weight, 20 parts of petroleum coke, 40 parts of an oxidizing agent, 40 parts of a reducing agent and 2 parts of a modifying agent.
3. The high-rate anode material according to claim 1, characterized in that: the composite material comprises, by weight, 40 parts of petroleum coke, 80 parts of an oxidizing agent, 80 parts of a reducing agent and 2 parts of a modifying agent.
4. The preparation method of the high-rate negative electrode material is characterized by comprising the following steps of:
s1, selecting granular petroleum coke as a petroleum carbon raw material, and crushing the petroleum carbon raw material;
s2, carrying out oxidation reduction treatment on the petroleum coke treated by the S1;
s21, oxidizing the petroleum coke treated by the S1 by using an oxidizing agent;
s22, reducing the petroleum coke treated by the S21 by using a reducing agent;
s3, the petroleum coke after the treatment of S2 is fluorinated and modified.
5. The method for preparing a high-rate anode material according to claim 1, wherein the step S1 comprises the following steps:
s11, mechanically crushing the petroleum carbon raw material by using a planetary ball mill and a ball milling medium, wherein the crushing grain size is within 15 mu m;
s12, in the course of S11, particle size analysis was performed using a laser particle size analyzer or SEM.
6. The method for preparing the high-rate negative electrode material as claimed in claim 2, wherein the ball-milling medium in S11 is ethanol.
7. The method for preparing a high-rate anode material according to claim 1, wherein the step S21 comprises the following steps:
s211, placing 1 part by weight of petroleum coke into a container, adding 2 parts by weight of oxidant to immerse the petroleum coke, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s212, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃.
8. The method for preparing a high-rate anode material according to claim 4, wherein the oxidant is H2O2、HNO3、H2SO4、KMnO4、K2Cr2O7。
9. The method for preparing a high-rate anode material according to claim 1, wherein the step S22 comprises the following steps:
s221, putting 1 part by weight of petroleum coke into a container, adding 2 parts by weight of reducing solution, and magnetically stirring at the ambient temperature of 20-25 ℃ for 4-5 hours;
s222, performing suction filtration by using a suction filtration device, and then placing the product in an oven for drying, wherein the drying temperature is 100 ℃.
10. The method for preparing a high-rate anode material according to claim 1, wherein the step S3 comprises the following steps:
s31, putting the petroleum coke with the mass ratio of 1 into a container, adding water with the mass ratio of 1.5 for dissolving and dispersing, and adding LINO with the mass ratio of 0.08-0.13Magnetically stirring for 2h at the ambient temperature of 20-25 ℃;
s32, adding modifier NH with the mass ratio of 0.04-0.054HF2Performing magnetic stirring for 8 hours, performing suction filtration by using a suction filtration device, placing the mixture in an oven for drying and grinding, wherein the temperature of a drying box is 100 ℃;
and S33, roasting the coated powder for 12 hours under the protection of nitrogen atmosphere, wherein the roasting temperature is 500 ℃, and thus obtaining a coated product.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014022041A (en) * | 2012-07-12 | 2014-02-03 | Sony Corp | Negative-electrode active material, manufacturing method thereof, lithium ion battery, battery pack, electronic device, electrically-powered vehicle, power storage device, and electric power system |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014022041A (en) * | 2012-07-12 | 2014-02-03 | Sony Corp | Negative-electrode active material, manufacturing method thereof, lithium ion battery, battery pack, electronic device, electrically-powered vehicle, power storage device, and electric power system |
Non-Patent Citations (1)
| Title |
|---|
| 谢一龙: "石油焦炭素作为锂离子电池负极材料的改性研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 02, pages 015 - 110 * |
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