CN112952069A - Production process of carbon-coated graphite negative electrode material - Google Patents
Production process of carbon-coated graphite negative electrode material Download PDFInfo
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- CN112952069A CN112952069A CN202110368230.3A CN202110368230A CN112952069A CN 112952069 A CN112952069 A CN 112952069A CN 202110368230 A CN202110368230 A CN 202110368230A CN 112952069 A CN112952069 A CN 112952069A
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- graphite
- carbon
- production process
- coated graphite
- drying
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 59
- 239000010439 graphite Substances 0.000 title claims abstract description 59
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000007773 negative electrode material Substances 0.000 title claims description 10
- 239000002608 ionic liquid Substances 0.000 claims abstract description 17
- 239000010406 cathode material Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- 239000000376 reactant Substances 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000012286 potassium permanganate Substances 0.000 claims description 10
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 10
- BSKSXTBYXTZWFI-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;acetate Chemical compound CC([O-])=O.CCCC[N+]=1C=CN(C)C=1 BSKSXTBYXTZWFI-UHFFFAOYSA-M 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 5
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 5
- 238000010000 carbonizing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000005011 phenolic resin Substances 0.000 claims description 5
- 229920001568 phenolic resin Polymers 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000010405 anode material Substances 0.000 claims 4
- 238000007599 discharging Methods 0.000 abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000003780 insertion Methods 0.000 abstract description 2
- 230000037431 insertion Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 229910052744 lithium Inorganic materials 0.000 description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 229910000733 Li alloy Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000001989 lithium alloy Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011255 nonaqueous electrolyte Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
Abstract
The invention discloses a production process of a carbon-coated graphite cathode material, which comprises the following steps of; the invention relates to the technical field of graphite cathode material processing, and the process has the advantages of simple operation and low cost, is beneficial to the insertion and the separation of lithium ions in the charging and discharging processes of graphite by oxidizing and pore-forming the graphite, and further improves the electrochemical performance of the graphite by coating a carbon source on the outer side of a graphite cathode through ionic liquid, improves the existing graphite cathode material, and brings convenience to people.
Description
Technical Field
The invention relates to the technical field of graphite cathode material processing, in particular to a production process of a carbon-coated graphite cathode material.
Background
The lithium battery is a primary battery which takes lithium metal or lithium alloy as a negative electrode material and uses a non-aqueous electrolyte solution, is different from a rechargeable battery, namely a lithium ion battery and a lithium ion polymer battery, and has very high requirements on the environment due to the processing, storage and use of the lithium metal because the chemical characteristics of the lithium metal are very active. Therefore, lithium batteries have not been used for a long time. With the development of microelectronic technology at the end of the twentieth century, miniaturized devices are increasing, and high requirements are made on power supplies. The lithium battery has then entered a large-scale practical stage.
At present, graphite is used as a common negative electrode material of a lithium battery, however, the traditional carbon-coated graphite negative electrode material is complex in preparation process and complex in operation, and the produced negative electrode material is not high in charging and discharging efficiency and inconvenient to use.
Disclosure of Invention
The invention aims to provide a production process of a carbon-coated graphite cathode material, which solves the problems of complex production process, complex operation and low charging and discharging efficiency of the carbon-coated graphite cathode material in the prior art.
The technical scheme of the invention is that the production process of the carbon-coated graphite cathode material comprises the following steps:
s1: preparing a potassium permanganate solution with the concentration of 3-8 mg/mL, adding graphite into the potassium permanganate solution, stirring to oxidize the graphite, forming holes on the surface of the graphite, filtering, washing for 2-3 times, and drying to obtain porous graphite;
s2: adding an organic solvent into a reaction kettle, adding phenolic resin for dissolving to form a solution with the concentration of 12-16 wt%, and then adding ionic liquid for mixing to obtain a mixed solution;
s3: adding the porous graphite obtained in the step S1 into the mixed solution of the step S2, raising the temperature in the reaction kettle to 50-60 ℃, introducing inert gas, and reacting for 2-3 hours to obtain a reactant;
s4: putting the reactant into a vacuum drying oven for drying;
s5: and (5) carbonizing the reactant dried in the step (S4) at 900-1800 ℃, continuing for 5-15 hours, cooling to room temperature, and crushing and sieving to obtain the carbon-coated graphite cathode material.
Preferably, the organic solvent is any one of trichloroethylene, carbon tetrachloride or ethanol.
Preferably, the ionic liquid in S2 is 1-butyl-3-methylimidazolium acetate.
Preferably, the mass percentage concentration of the ionic liquid is 2 wt% -8 wt%.
Preferably, the inert gas in step S3 is any one of nitrogen and argon.
Preferably, in the step S4, the drying temperature is 45-50 ℃, and the drying time is 18-22 h.
The invention has the beneficial effects that:
the process is simple to operate and low in cost, and the graphite is oxidized to form pores, so that the graphite is favorable for the insertion and the separation of lithium ions in the charging and discharging process, the charging and discharging efficiency is improved, and meanwhile, the carbon source is coated on the outer side of the graphite cathode through the ionic liquid, so that the electrochemical performance of the graphite is further improved, the existing graphite cathode material is improved, and convenience is brought to the use of people.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A production process of a carbon-coated graphite negative electrode material comprises the following steps:
s1: preparing a potassium permanganate solution with the concentration of 3mg/mL, adding graphite into the potassium permanganate solution, stirring the solution to oxidize the graphite, forming holes on the surface of the graphite, filtering, washing for 2 times, and drying to obtain porous graphite;
s2: adding an organic solvent into a reaction kettle, wherein the organic solvent is any one of trichloroethylene, carbon tetrachloride or ethanol, adding phenolic resin for dissolving to form a 12 wt% solution, adding an ionic liquid for mixing, and the ionic liquid is 1-butyl-3-methylimidazolium acetate, and the mass percentage concentration of the ionic liquid is 2 wt%, so as to obtain a mixed solution;
s3: adding the porous graphite obtained in the step S1 into the mixed solution of the step S2, raising the temperature in the reaction kettle to 50 ℃, introducing nitrogen, and reacting for 2 hours to obtain a reactant;
s4: putting the reactant into a vacuum drying oven for drying at the drying temperature of 45 ℃ for 18 h;
s5: and (4) carbonizing the reactant dried in the step (S4) at 900 ℃ for 5 hours, cooling to room temperature, crushing and sieving to obtain the carbon-coated graphite cathode material.
Example 2
A production process of a carbon-coated graphite negative electrode material comprises the following steps:
s1: preparing a potassium permanganate solution with the concentration of 6mg/mL, adding graphite into the potassium permanganate solution, stirring the solution to oxidize the graphite, forming holes on the surface of the graphite, filtering, washing for 3 times, and drying to obtain porous graphite;
s2: adding an organic solvent into a reaction kettle, wherein the organic solvent is any one of trichloroethylene, carbon tetrachloride or ethanol, adding phenolic resin to dissolve the organic solvent to form a 14 wt% solution, adding an ionic liquid, and mixing, wherein the ionic liquid is 1-butyl-3-methylimidazolium acetate, and the mass percentage concentration of the ionic liquid is 5 wt%, so as to obtain a mixed solution;
s3: adding the porous graphite obtained in the step S1 into the mixed solution of the step S2, raising the temperature in the reaction kettle to 55 ℃, introducing nitrogen, and reacting for 2 hours to obtain a reactant;
s4: putting the reactant into a vacuum drying oven for drying at the drying temperature of 50 ℃ for 20 hours;
s5: and (4) carbonizing the reactant dried in the step S4 at 1300 ℃ for 10 hours, cooling to room temperature, crushing and sieving to obtain the carbon-coated graphite cathode material.
Example 3
A production process of a carbon-coated graphite negative electrode material comprises the following steps:
s1: preparing a potassium permanganate solution with the concentration of 8mg/mL, adding graphite into the potassium permanganate solution, stirring to oxidize the graphite, forming holes on the surface of the graphite, filtering, washing for 3 times, and drying to obtain porous graphite;
s2: adding an organic solvent into a reaction kettle, wherein the organic solvent is any one of trichloroethylene, carbon tetrachloride or ethanol, adding phenolic resin to dissolve the organic solvent to form a 16 wt% solution, adding an ionic liquid, and mixing, wherein the ionic liquid is 1-butyl-3-methylimidazolium acetate, and the mass percentage concentration of the ionic liquid is 8 wt%, so as to obtain a mixed solution;
s3: adding the porous graphite obtained in the step S1 into the mixed solution of the step S2, raising the temperature in the reaction kettle to 60 ℃, introducing nitrogen, and reacting for 3 hours to obtain a reactant;
s4: putting the reactant into a vacuum drying oven for drying at the drying temperature of 50 ℃ for 22 h;
s5: and (4) carbonizing the dried reactant obtained in the step S4 at 1800 ℃ for 15 hours, cooling to room temperature, and crushing and sieving to obtain the carbon-coated graphite cathode material.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. A production process of a carbon-coated graphite negative electrode material is characterized by comprising the following steps:
s1: preparing a potassium permanganate solution with the concentration of 3-8 mg/mL, adding graphite into the potassium permanganate solution, stirring to oxidize the graphite, forming holes on the surface of the graphite, filtering, washing for 2-3 times, and drying to obtain porous graphite;
s2: adding an organic solvent into a reaction kettle, adding phenolic resin for dissolving to form a solution with the concentration of 12-16 wt%, and then adding ionic liquid for mixing to obtain a mixed solution;
s3: adding the porous graphite obtained in the step S1 into the mixed solution of the step S2, raising the temperature in the reaction kettle to 50-60 ℃, introducing inert gas, and reacting for 2-3 hours to obtain a reactant;
s4: putting the reactant into a vacuum drying oven for drying;
s5: and (5) carbonizing the reactant dried in the step (S4) at 900-1800 ℃, continuing for 5-15 hours, cooling to room temperature, and crushing and sieving to obtain the carbon-coated graphite cathode material.
2. The process for producing a carbon-coated graphite anode material according to claim 1, wherein the organic solvent is any one of trichloroethylene, carbon tetrachloride or ethanol.
3. The production process of the carbon-coated graphite anode material as claimed in claim 2, wherein the ionic liquid in S2 is 1-butyl-3-methylimidazolium acetate.
4. The production process of the carbon-coated graphite anode material as claimed in claim 3, wherein the mass percentage concentration of the ionic liquid is 2 wt% -8 wt%.
5. The process of claim 4, wherein the inert gas in step S3 is any one of nitrogen and argon.
6. The production process of the carbon-coated graphite anode material according to claim 1, wherein in the step S4, the drying temperature is 45-50 ℃ and the drying time is 18-22 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110368230.3A CN112952069A (en) | 2021-04-06 | 2021-04-06 | Production process of carbon-coated graphite negative electrode material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110368230.3A CN112952069A (en) | 2021-04-06 | 2021-04-06 | Production process of carbon-coated graphite negative electrode material |
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|---|---|
| CN112952069A true CN112952069A (en) | 2021-06-11 |
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|---|---|---|---|
| CN202110368230.3A Pending CN112952069A (en) | 2021-04-06 | 2021-04-06 | Production process of carbon-coated graphite negative electrode material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104882609A (en) * | 2015-04-20 | 2015-09-02 | 洛阳月星新能源科技有限公司 | Surface modification treatment method for negative electrode graphite in low-temperature lithium ion battery |
| CN104934579A (en) * | 2015-05-22 | 2015-09-23 | 田东 | Preparation method for porous graphite doped and carbon coated graphite anode material |
| CN106684360A (en) * | 2017-01-20 | 2017-05-17 | 江西紫宸科技有限公司 | Carbon coating method of artificial graphite negative material, negative material and lithium ion battery |
-
2021
- 2021-04-06 CN CN202110368230.3A patent/CN112952069A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104882609A (en) * | 2015-04-20 | 2015-09-02 | 洛阳月星新能源科技有限公司 | Surface modification treatment method for negative electrode graphite in low-temperature lithium ion battery |
| CN104934579A (en) * | 2015-05-22 | 2015-09-23 | 田东 | Preparation method for porous graphite doped and carbon coated graphite anode material |
| CN106684360A (en) * | 2017-01-20 | 2017-05-17 | 江西紫宸科技有限公司 | Carbon coating method of artificial graphite negative material, negative material and lithium ion battery |
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Application publication date: 20210611 |
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