CN111268677A - Preparation method and application of novel lithium ion battery negative electrode material carbonized grape seed - Google Patents
Preparation method and application of novel lithium ion battery negative electrode material carbonized grape seed Download PDFInfo
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/342—Preparation characterised by non-gaseous activating agents
- C01B32/348—Metallic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a preparation method and application of a novel lithium ion battery negative electrode material carbonized grape seed. Drying grape seeds, grinding the grape seeds into powder, soaking the powder in an activating agent solution, and magnetically stirring the powder for 4 hours at the temperature of 80 ℃; filtering, vacuum drying the soaked grape seed powder at 80 ℃ for 12h, then placing the grape seed powder in a tube furnace, calcining the grape seed powder at 700 ℃ and 900 ℃ for 2-6h under the argon atmosphere, cooling to room temperature, sequentially using hydrochloric acid and distilled water to centrifugally wash the grape seed powder to be neutral, vacuum drying and grinding the grape seed powder to obtain the target product carbonized grape seed. According to the invention, the carbonized grape seeds are used as the lithium ion battery cathode material, on one hand, the raw materials are easy to obtain and are green and environment-friendly, and on the other hand, the carbonized grape seeds have a porous structure, so that the active sites of the reaction are increased, the conductivity of the material can be improved, and the electrochemical performance of the material is improved.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a preparation method and application of a novel lithium ion battery negative electrode material carbonized grape seed.
Background
Since the market for lithium ion batteries in the 90's of the 20 th century, they were consistently favored by the battery industry and users for their excellent electrochemical performance. At present, the lithium ion battery has a leading position in the fields of mobile electronic terminal equipment such as notebook computers, mobile phones, cameras and the like, and has great application prospect and commercial value in the fields of new energy resources such as power automobiles and the like.
The electrode active material is the core of the battery and plays a decisive role in the battery performance. Carbon materials have been considered as the most commercially valuable anode materials in LIBs. The carbon material selected by the current commercial rechargeable lithium battery cathode is generally graphite which is used as a lithium ion battery cathode material and has good conductivity and excellent cycling stability; the non-renewable, low theoretical capacity and diffusion coefficient of lithium ions of graphite, however, limit its application in power sources with high energy and power density requirements, such as electric vehicles. In order to solve these problems, researchers have studied carbon nanotubes and other carbonaceous materials having higher performance by generating additional lithium ion sites. However, their large-scale application is limited by the non-regenerability and high cost of carbon precursors and the complex manufacturing techniques. The energy shortage and growing market demand still drives researchers to find inexhaustible and effective resources for the production of high performance carbonaceous materials.
In recent years, the biomass porous carbon material has attracted extensive attention of researchers due to the advantages of low cost, abundant microstructure, reproducibility, environmental friendliness and the like. In addition, as an electrode material of a lithium ion battery, the lithium ion battery should have a high capacity, excellent rate capability and good cycle stability.
At present, research on biomass porous carbon materials has attracted more and more attention from scientific researchers and industrial circles at home and abroad. The treatment of the waste grape seeds is a big problem because the yield of grapes in China is quite high, in addition, the grape seeds are rich in carbon-containing compounds such as grape seed oil, lignin and cellulose, the carbon content is high, the cost is greatly reduced after the waste biomass is used as an electrode material for energy storage equipment to improve the capacity, and a green environment can be created. At present, no report exists that grape seeds are used as raw materials to prepare a three-dimensional porous carbon material and the three-dimensional porous carbon material is applied to the field of lithium ion battery cathodes.
Disclosure of Invention
The invention aims to provide a preparation method and application of a novel lithium ion battery negative electrode material carbonized grape seed to improve the electrochemical performance of a lithium ion battery.
The technical scheme provided by the invention is as follows: a preparation method of a novel lithium ion battery negative electrode material carbonized grape seed comprises the following steps: drying grape seeds, grinding the grape seeds into powder, soaking the powder in an activating agent solution, and magnetically stirring the powder for 4 hours at the temperature of 80 ℃; filtering, vacuum drying the soaked grape seed powder at 80 ℃ for 12h, then placing the grape seed powder in a tube furnace, calcining the grape seed powder at 700 ℃ and 900 ℃ for 2-6h under the argon atmosphere, cooling to room temperature, sequentially using hydrochloric acid and distilled water to centrifugally wash the grape seed powder to be neutral, vacuum drying and grinding the grape seed powder to obtain the target product carbonized grape seed.
Further, in the above preparation method, the activator solution is a potassium hydroxide solution.
Further, according to the preparation method, the grape seed powder and the potassium hydroxide are 1:1-4 in mass ratio.
Further, in the preparation method, the calcining temperature is 800 ℃.
Further, in the preparation method, the calcination time is 3 hours.
The invention provides application of carbonized grape seeds as a negative electrode material in a lithium ion battery.
Further, the application and the method are as follows: uniformly stirring a negative electrode material, a binder and a conductive agent, and coating the mixture on a copper foil to be used as a negative electrode of the lithium ion battery; the negative electrode material is carbonized grape seeds.
Further, in the above application, the conductive agent is acetylene black, and the binder is PVDF (polyvinylidene fluoride).
Further, according to the application, the carbonized grape seeds comprise acetylene black, PVDF (6-8), PVDF (3-1) and 1 in weight ratio.
Further, the carbonized grape seed comprises acetylene black and PVDF in a weight ratio of 6:3:1, 7:2:1 or 8:1: 1.
The invention has the beneficial effects that:
1. the method takes grape seeds as raw materials, potassium hydroxide as an activating agent, and obtains carbonized grape seeds by magnetic stirring in an oil bath kettle at 80 ℃ for 4 hours, vacuum drying and high-temperature calcination.
2. The method for preparing the carbonized grape seeds from the natural grape seeds has the characteristics of easily obtained raw materials, environmental protection, sustainability and the like, and the prepared material has high carbon content and a uniform porous structure. The formation of the pore structure not only increases the lithium ion storage capacity but also reduces the resistance to lithium ion migration and accelerates the migration speed during charge and discharge thereof. And can make the material more compatible with the electrolyte.
3. The grape seeds are rich in carbon-containing compounds such as grape seed oil, lignin, cellulose and the like, and the carbon content is high.
4. The invention prepares the three-dimensional porous carbon material by a chemical activation method, and the simple and economic preparation method provides a foundation for further industrial application of the waste biomass.
Drawings
FIG. 1 is an SEM image of carbonized grape seeds prepared according to the present invention.
FIG. 2 is an XRD pattern of carbonized grape seeds prepared in accordance with the present invention.
FIG. 3 is a Raman image of carbonized grape seeds prepared in accordance with the present invention.
Detailed Description
The invention is further explained below with reference to specific embodiments, but is not intended to limit the scope of protection of the invention.
In order to improve the electrochemical performance of the lithium ion battery and find a suitable substitute of the negative electrode material graphite, the invention provides a preparation method and application of a negative electrode material carbonized grape seed of the lithium ion battery, which comprises the following steps:
1) dissolving potassium hydroxide in distilled water at room temperature to prepare a potassium hydroxide solution;
preferably, the concentration of the potassium hydroxide solution is 60-100 mg/mL.
More preferably, the concentration of the potassium hydroxide solution is 80 mg/mL.
2) Drying grape seeds, grinding the grape seeds into powder, soaking the grape seed powder in a potassium hydroxide solution, magnetically stirring the grape seed powder in an oil bath kettle at the temperature of 80 ℃ for 4 hours, filtering the grape seed powder, and drying the soaked grape seed powder at the temperature of 80 ℃ in vacuum for 12 hours;
preferably, the weight ratio of the grape seed powder to the potassium hydroxide is 1: 1-4.
3) Placing the grape seed powder dried in the step 2) in a tube furnace, calcining for 2-6h at the temperature of 700-900 ℃ in the argon atmosphere, cooling to room temperature, sequentially centrifugally washing to neutrality by using hydrochloric acid and distilled water, drying for 12h in vacuum at the temperature of 80 ℃, and grinding to obtain the target product carbonized grape seeds.
Preferably, the calcination temperature is 800 ℃ and the calcination time is 3 h.
In the present invention, the potassium hydroxide solution is prepared so as to be enriched with K+. Magnetically stirring grape seed powder in potassium hydroxide solution at 80 deg.C for 4 hr to make K+The porous carbonized grape seed material can be added into grape seed powder to prepare porous carbonized grape seed material.
Example 1 lithium ion Battery negative electrode Material carbonized grape seed
The preparation method comprises the following steps:
1) a potassium hydroxide solution having a concentration of 80mg/mL was prepared by dissolving 4g of potassium hydroxide in 50mL of distilled water at room temperature and stirring.
2) Drying grape seeds, grinding the grape seeds into powder, adding 1.5g of grape seed powder into the potassium hydroxide solution obtained in the step 1), soaking, magnetically stirring for 4 hours in an oil bath kettle at 80 ℃, filtering, and vacuum-drying the soaked grape seed powder for 12 hours at 80 ℃.
3) Placing the grape seed powder dried in the step 2) in a tube furnace, calcining for 3h at 800 ℃ in an argon atmosphere, cooling the obtained product to room temperature, then sequentially centrifugally washing with hydrochloric acid and distilled water to neutrality, vacuum drying for 12h at 80 ℃, and grinding to obtain the target product carbonized grape seeds.
(II) detection
Fig. 1 is an SEM image of the prepared carbonized grape seeds, and it can be seen from fig. 1 that the carbonized grape seed material prepared by the present invention has a cellular porous structure.
Fig. 2 is an XRD pattern of the prepared carbonized grape seeds, and it can be seen from fig. 2 that there is a peak at 26 ° 2 θ, which is consistent with XRD patterns reported in the literature for graphite carbon materials.
FIG. 3 is a Raman spectrum of the prepared carbonized grape seeds. As can be seen from FIG. 3, the carbonized grape seeds were found to be 1350cm in length-1、1595cm-1There are D and G peaks, consistent with the Raman spectrum of the graphitic carbon material.
As can be seen from fig. 1, 2 and 3, the carbonized grape seed material obtained by the present invention has a graphene-like porous honeycomb material and a uniform pore structure.
Example 2 application of carbonized grape seeds as negative electrode material of lithium ion battery
Assembly of lithium ion battery
1) Common acetylene black purchased from the market is taken as a conductive agent, PVDF is taken as a binder, and carbonized grape seeds prepared in example 1 are taken as a negative electrode material. According to the mass ratio, the carbonized grape seeds, the acetylene black and the PVDF are mixed and pasted, the mixture is uniformly coated on a copper foil to be used as a negative electrode, and a lithium sheet is used as a positive electrode to assemble the button cell-1.
2) Common acetylene black purchased from the market is taken as a conductive agent, PVDF is taken as a binder, and carbonized grape seeds prepared in example 1 are taken as a negative electrode material. According to the weight ratio, carbonized grape seeds, acetylene black and PVDF (polyvinylidene fluoride) are mixed and pasted, the mixture is uniformly coated on a copper foil to serve as a negative electrode, and a lithium sheet is used as a positive electrode to assemble a button cell-2.
3) Common acetylene black purchased from the market is taken as a conductive agent, PVDF is taken as a binder, and the grape seeds carbide prepared in example 1 is taken as a negative electrode material, the grape seeds carbide, the acetylene black and the PVDF are mixed and pasted according to the weight ratio, the mixture is uniformly coated on a copper foil to be taken as a negative electrode, and a (lithium sheet) is taken as a positive electrode to assemble the button cell-3.
Comparative example: common acetylene black purchased from the market is taken as a conductive agent, PVDF is taken as a binder, graphite is taken as a negative electrode material, the materials are mixed and pasted according to the mass ratio of 7:2:1, the mixture is uniformly coated on copper foil to be taken as a negative electrode, and a (lithium sheet) is taken as a positive electrode to assemble the button cell-4.
(II) electrochemical Performance testing
Electrochemical tests were carried out on button cells prepared with different amounts of negative electrode materials, and the results are shown in table 1.
TABLE 1 comparison of electrochemical Performance of batteries made with different negative electrode materials (Current Density 0.1A/g)
As can be seen from table 1, compared with the graphite negative electrode material, the electrochemical performance of the carbonized grape seed synthesized by the method of the present invention as the negative electrode material is significantly improved, and with the increase of the quality of the carbonized grape seed, the electrochemical performance of the negative electrode material synthesized by the method of the present invention is firstly improved and then weakened, and it can be seen that the electrochemical performance of the battery material prepared by the carbonized grape seed, acetylene black and PVDF in a mass ratio of 7:2:1 is significantly higher than that of the material obtained under other conditions, on the premise of maintaining the excellent characteristics of the negative electrode material, the reversible capacity of the battery is increased, the electrochemical performance of the material is improved, and the raw material is natural grape seed, which is green, environment-friendly and easy to obtain.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a novel lithium ion battery negative electrode material carbonized grape seed is characterized by comprising the following steps: drying grape seeds, grinding the grape seeds into powder, soaking the powder in an activating agent solution, and magnetically stirring the powder for 4 hours at the temperature of 80 ℃; filtering, vacuum drying the soaked grape seed powder at 80 ℃ for 12h, then placing the grape seed powder in a tube furnace, calcining the grape seed powder at 700 ℃ and 900 ℃ for 2-6h under the argon atmosphere, cooling to room temperature, sequentially using hydrochloric acid and distilled water to centrifugally wash the grape seed powder to be neutral, vacuum drying and grinding the grape seed powder to obtain the target product carbonized grape seed.
2. The method of claim 1, wherein the activator solution is a potassium hydroxide solution.
3. The method according to claim 2, wherein the ratio of the grape seed powder to the potassium hydroxide is 1:1-4 by mass.
4. The process according to claim 1, wherein the calcination temperature is 800 ℃.
5. The process according to claim 1, wherein the calcination is carried out for a period of 3 hours.
6. Use of carbonized grape seeds prepared according to the method of any one of claims 1 to 5 as negative electrode material in lithium ion batteries.
7. Use according to claim 6, characterized in that the method is as follows: uniformly stirring a negative electrode material, a binder and a conductive agent, and coating the mixture on a copper foil to be used as a negative electrode of the lithium ion battery; the negative electrode material is carbonized grape seeds prepared by the method of any one of claims 1 to 5.
8. Use according to claim 7, wherein the conductive agent is acetylene black and the binder is PVDF.
9. The use according to claim 8, wherein the carbonized grape seed comprises, by weight, acetylene black PVDF (6-8): 3-1): 1.
10. Use according to claim 9, wherein the carbonized grape seed is at a weight ratio of acetylene black to PVDF 6:3:1, 7:2:1 or 8:1: 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112736243A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Preparation method and application of novel lithium ion battery negative electrode material carbonized grape skin |
| CN112736234A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Novel lithium ion battery cathode material based on biomass/carbon nanotube composite modified lithium titanate and application thereof |
| CN112736236A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Novel biomass carbon-coated biphase Li serving as lithium ion battery negative electrode material4Ti5O12-TiO2And uses thereof |
| CN112736235A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Biomass/carbon nanotube induced Fe3O4Nano composite material and application thereof as negative electrode material of lithium ion battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112736243A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Preparation method and application of novel lithium ion battery negative electrode material carbonized grape skin |
| CN112736234A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Novel lithium ion battery cathode material based on biomass/carbon nanotube composite modified lithium titanate and application thereof |
| CN112736236A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Novel biomass carbon-coated biphase Li serving as lithium ion battery negative electrode material4Ti5O12-TiO2And uses thereof |
| CN112736235A (en) * | 2021-01-15 | 2021-04-30 | 辽宁大学 | Biomass/carbon nanotube induced Fe3O4Nano composite material and application thereof as negative electrode material of lithium ion battery |
| CN112736235B (en) * | 2021-01-15 | 2024-02-20 | 辽宁大学 | Biomass/carbon nanotube induced Fe 3 O 4 Nanocomposite and application thereof as lithium ion battery anode material |
| CN112736234B (en) * | 2021-01-15 | 2024-02-20 | 辽宁大学 | Novel lithium ion battery anode material based on biomass/carbon nanotube composite modified lithium titanate and application thereof |
| CN112736236B (en) * | 2021-01-15 | 2024-02-20 | 辽宁大学 | Novel lithium ion battery anode material biomass carbon coated diphasic Li 4 Ti 5 O 12 -TiO 2 And applications thereof |
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