CN107863527B - Composite negative electrode material and preparation method and application thereof - Google Patents
Composite negative electrode material and preparation method and application thereof Download PDFInfo
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- CN107863527B CN107863527B CN201710927689.6A CN201710927689A CN107863527B CN 107863527 B CN107863527 B CN 107863527B CN 201710927689 A CN201710927689 A CN 201710927689A CN 107863527 B CN107863527 B CN 107863527B
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- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 239000007773 negative electrode material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000002156 mixing Methods 0.000 claims abstract description 51
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 50
- 239000010439 graphite Substances 0.000 claims abstract description 50
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000003756 stirring Methods 0.000 claims abstract description 39
- 239000003822 epoxy resin Substances 0.000 claims abstract description 22
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 22
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000967 suction filtration Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 45
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000007873 sieving Methods 0.000 claims description 15
- 239000010405 anode material Substances 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 13
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000002441 reversible effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 101150047356 dec-1 gene Proteins 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910032387 LiCoO2 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000001166 ammonium sulphate Substances 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- CSNNHWWHGAXBCP-UHFFFAOYSA-L magnesium sulphate Substances [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000001120 potassium sulphate Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000012360 testing method Methods 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
- H01M4/58—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
- 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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a composite negative electrode material and a preparation method and application thereof, wherein the composite negative electrode material comprises the following raw materials in parts by weight: 31-39 parts of graphite tailings, 3-7 parts of yttrium nitrate, 13-21 parts of chloroplatinic acid, 515-12 parts of epoxy resin E, 3-7 parts of diethylenetriamine and 10-20 parts of graphite. Mixing and grinding graphite tailings and yttrium nitrate, mixing with a chloroplatinic acid solution, heating and stirring; then adding a diethylenetriamine solution, heating and stirring, then carrying out suction filtration, washing and drying, then uniformly mixing with graphite, crushing, mixing with epoxy resin E51, and calcining to obtain the epoxy resin. The prepared negative electrode material has good electrochemical performance, and can improve the reversible specific capacity, the charge-discharge efficiency, the cycle performance stability and the rate performance of the lithium ion battery; the method can also recycle the graphite tailings, has extremely obvious effect and simple preparation process, and is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a composite negative electrode material and a preparation method and application thereof.
Background
Compared with the traditional lead-acid and nickel-cadmium secondary batteries, the lithium ion battery has the advantages of high working voltage, high specific energy, wide working temperature range, stable discharge, long cycle life, no memory effect and the like, so that the lithium ion battery serving as a novel energy storage power supply is widely applied to the fields of communication equipment, electric tools, aerospace and the like.
With the continuous progress of the technology, people put forward higher requirements on lithium ion batteries, and the lithium ion batteries with the performances of high energy density, high rate performance, long cycle life, high safety coefficient and the like gradually become research hotspots of people. Graphite is the main commercial carbon negative electrode material of the lithium ion battery at present. The graphene is also paid more and more attention, but the graphite and the graphene are expensive and are limited in application. The graphite tailings are low in cost, occupy a large amount of earth surface, damage the land, and are very easy to cause landslide and debris flow accidents, but the graphite tailings have poor effect in batteries, cannot be directly used and need to be treated.
Disclosure of Invention
The invention aims to provide a composite negative electrode material, a preparation method and application thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a composite negative electrode material comprises the following raw materials in parts by weight: 31-39 parts of graphite tailings, 3-7 parts of yttrium nitrate, 13-21 parts of chloroplatinic acid, 515-12 parts of epoxy resin E, 3-7 parts of diethylenetriamine and 10-20 parts of graphite.
As a further scheme of the invention: the composite negative electrode material comprises the following raw materials in parts by weight: 33-37 parts of graphite tailings, 4-6 parts of yttrium nitrate, 15-19 parts of chloroplatinic acid, 517-10 parts of epoxy resin E, 4-6 parts of diethylenetriamine and 12-18 parts of graphite.
As a further scheme of the invention: the composite negative electrode material comprises the following raw materials in parts by weight: 35 parts of graphite tailings, 5 parts of yttrium nitrate, 17 parts of chloroplatinic acid, 518 parts of epoxy resin E, 5 parts of diethylenetriamine and 15 parts of graphite.
A preparation method of the composite anode material comprises the following steps:
1) mixing chloroplatinic acid with deionized water with the mass of 7.5-8 times of that of the chloroplatinic acid to prepare a chloroplatinic acid solution; mixing diethylenetriamine with deionized water in an amount of 4.5 to 5 times the mass of the diethylenetriamine to prepare a diethylenetriamine solution;
2) mixing and grinding the graphite tailings and yttrium nitrate, sieving the mixture through a sieve with the temperature of 100-150 meshes, then mixing the mixture with a chloroplatinic acid solution, heating to the temperature of 58-60 ℃, stirring for 50-60min at the temperature, heating to the temperature of 120-125 ℃, and sealing and stirring for 25-30min at the temperature; then adding diethylenetriamine solution, stirring for 1.5-1.8h at the temperature of 80-82 ℃, and then performing suction filtration, washing and drying to obtain a mixture A;
3) and uniformly mixing the mixture A and graphite, crushing the mixture, sieving the mixture by a sieve with 120-fold sand and 150 meshes, uniformly mixing the mixture A and the epoxy resin E51, calcining the mixture for 5.5 to 6 hours at the temperature of 500 ℃ in a protective atmosphere, and calcining the mixture for 8 to 10 hours at the temperature of 1500-fold sand and 1600 ℃ to obtain the catalyst.
As a further scheme of the invention: the protective atmosphere adopts one of helium, nitrogen and argon.
As a further scheme of the invention: in the step 2), the stirring speed after mixing with the chloroplatinic acid solution is 250-300 r/min.
As a further scheme of the invention: in the step 2), the stirring speed after adding the diethylenetriamine solution is 180-200 r/min.
The invention also aims to provide application of the composite negative electrode material in a battery.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the chloroplatinic acid and diethylenetriamine are adopted to treat the graphite tailings, and the negative electrode material prepared by other processes has good electrochemical performance, and can improve the reversible specific capacity, the charge-discharge efficiency, the cycle performance stability and the rate capability of the lithium ion battery; the method can also recycle the graphite tailings, has extremely obvious effect, simple preparation process, convenient operation, wide raw material source and low cost, and is suitable for large-scale industrial production. Can be used as a new cathode material applied to the field of lithium ion batteries and has excellent electrochemical performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
In an embodiment of the invention, the composite anode material comprises the following raw materials: 31kg of graphite tailings, 3kg of yttrium nitrate, 13kg of chloroplatinic acid, epoxy resin E515 kg, 3kg of diethylenetriamine and 10kg of graphite.
Mixing chloroplatinic acid with deionized water with the mass of which is 7.5 times that of the chloroplatinic acid to prepare a chloroplatinic acid solution; diethylene triamine was mixed with deionized water in an amount of 4.5 times the mass of the mixture to prepare a diethylene triamine solution. Mixing and grinding graphite tailings and yttrium nitrate, sieving the mixture by a 100-mesh sieve, mixing the mixture with a chloroplatinic acid solution, heating to 58 ℃, stirring at the temperature for 50min, heating to 120 ℃, and sealing and stirring at the temperature for 25 min; wherein the stirring speed after mixing with the chloroplatinic acid solution is 250 r/min. Then adding a diethylenetriamine solution, stirring at the temperature of 80 ℃ for 1.5h, and then carrying out suction filtration, washing and drying to obtain a mixture A; the stirring speed after the addition of the diethylenetriamine solution was 180 r/min. And uniformly mixing the mixture A and graphite, crushing, sieving by a 120-mesh sieve, uniformly mixing with epoxy resin E51, calcining for 5.5 hours at 500 ℃ in a helium atmosphere, and calcining for 8 hours at 1500 ℃.
Example 2
In an embodiment of the invention, the composite anode material comprises the following raw materials: 39kg of graphite tailings, 7kg of yttrium nitrate, 21kg of chloroplatinic acid, epoxy resin E5112 kg, 7kg of diethylenetriamine and 20kg of graphite.
Mixing chloroplatinic acid with deionized water with the mass of the chloroplatinic acid being 8 times that of the chloroplatinic acid to prepare a chloroplatinic acid solution; diethylene triamine was mixed with deionized water in an amount of 5 times the mass of the mixture to prepare a diethylene triamine solution. Mixing and grinding graphite tailings and yttrium nitrate, sieving the mixture by a 150-mesh sieve, mixing the mixture with a chloroplatinic acid solution, heating to 60 ℃, stirring at the temperature for 60min, heating to 125 ℃, and sealing and stirring at the temperature for 30 min; wherein the stirring speed after mixing with the chloroplatinic acid solution is 300 r/min. Then adding a diethylenetriamine solution, stirring at the temperature of 82 ℃ for 1.8h, and then carrying out suction filtration, washing and drying to obtain a mixture A; the stirring speed after the addition of the diethylenetriamine solution was 200 r/min. And uniformly mixing the mixture A and graphite, crushing, sieving by a 150-mesh sieve, uniformly mixing with epoxy resin E51, calcining for 6 hours at 500 ℃ in an argon atmosphere, and calcining for 10 hours at 1600 ℃.
Example 3
In an embodiment of the invention, the composite anode material comprises the following raw materials: 33kg of graphite tailings, 4kg of yttrium nitrate, 15kg of chloroplatinic acid, epoxy resin E517 kg, 4kg of diethylenetriamine and 12kg of graphite.
Mixing chloroplatinic acid with deionized water with the mass of the chloroplatinic acid being 8 times that of the chloroplatinic acid to prepare a chloroplatinic acid solution; diethylene triamine was mixed with deionized water in an amount of 5 times the mass of the mixture to prepare a diethylene triamine solution. Mixing and grinding graphite tailings and yttrium nitrate, sieving the mixture by a 120-mesh sieve, mixing the mixture with a chloroplatinic acid solution, heating to 59 ℃, stirring at the temperature for 55min, heating to 122 ℃, and sealing and stirring at the temperature for 30 min; wherein the stirring speed after mixing with the chloroplatinic acid solution is 280 r/min. Then adding a diethylenetriamine solution, stirring at the temperature of 81 ℃ for 1.8h, and then carrying out suction filtration, washing and drying to obtain a mixture A; the stirring speed after the addition of the diethylenetriamine solution was 200 r/min. And uniformly mixing the mixture A and graphite, crushing, sieving by a 150-mesh sieve, uniformly mixing with epoxy resin E51, calcining for 6 hours at 500 ℃ in a nitrogen atmosphere, and calcining for 10 hours at 1600 ℃.
Example 4
In an embodiment of the invention, the composite anode material comprises the following raw materials: 37kg of graphite tailings, 6kg of yttrium nitrate, 19kg of chloroplatinic acid, epoxy resin E5110 kg, 6kg of diethylenetriamine and 18kg of graphite.
Mixing chloroplatinic acid with deionized water with the mass of the chloroplatinic acid being 8 times that of the chloroplatinic acid to prepare a chloroplatinic acid solution; diethylene triamine was mixed with deionized water in an amount of 5 times the mass of the mixture to prepare a diethylene triamine solution. Mixing and grinding graphite tailings and yttrium nitrate, sieving the mixture by a 120-mesh sieve, mixing the mixture with a chloroplatinic acid solution, heating to 59 ℃, stirring at the temperature for 55min, heating to 122 ℃, and sealing and stirring at the temperature for 30 min; wherein the stirring speed after mixing with the chloroplatinic acid solution is 280 r/min. Then adding a diethylenetriamine solution, stirring at the temperature of 81 ℃ for 1.8h, and then carrying out suction filtration, washing and drying to obtain a mixture A; the stirring speed after the addition of the diethylenetriamine solution was 200 r/min. And uniformly mixing the mixture A and graphite, crushing, sieving by a 150-mesh sieve, uniformly mixing with epoxy resin E51, calcining for 6 hours at 500 ℃ in a nitrogen atmosphere, and calcining for 10 hours at 1600 ℃.
Example 5
In an embodiment of the invention, the composite anode material comprises the following raw materials: 35kg of graphite tailings, 5kg of yttrium nitrate, 17kg of chloroplatinic acid, epoxy resin E518 kg, 5kg of diethylenetriamine and 15kg of graphite.
Mixing chloroplatinic acid with deionized water with the mass of the chloroplatinic acid being 8 times that of the chloroplatinic acid to prepare a chloroplatinic acid solution; diethylene triamine was mixed with deionized water in an amount of 5 times the mass of the mixture to prepare a diethylene triamine solution. Mixing and grinding graphite tailings and yttrium nitrate, sieving the mixture by a 120-mesh sieve, mixing the mixture with a chloroplatinic acid solution, heating to 59 ℃, stirring at the temperature for 55min, heating to 122 ℃, and sealing and stirring at the temperature for 30 min; wherein the stirring speed after mixing with the chloroplatinic acid solution is 280 r/min. Then adding a diethylenetriamine solution, stirring at the temperature of 81 ℃ for 1.8h, and then carrying out suction filtration, washing and drying to obtain a mixture A; the stirring speed after the addition of the diethylenetriamine solution was 200 r/min. And uniformly mixing the mixture A and graphite, crushing, sieving by a 150-mesh sieve, uniformly mixing with epoxy resin E51, calcining for 6 hours at 500 ℃ in a nitrogen atmosphere, and calcining for 10 hours at 1600 ℃.
Comparative example 1
The starting materials and process were identical to those of example 5 except that chloroplatinic acid, diethylenetriamine, was not included.
Comparative example 2
Directly mixing graphite tailings, yttrium nitrate, chloroplatinic acid and diethylenetriamine, adding deionized water (the addition amount of the deionized water is consistent with that in example 5), stirring at the temperature of 81 ℃ for 1.8 hours, and then performing suction filtration, washing and drying to obtain a mixture A; the stirring speed was 200 r/min. And uniformly mixing the mixture A and graphite, crushing, sieving by a 150-mesh sieve, uniformly mixing with epoxy resin E51, calcining for 6 hours at 500 ℃ in a nitrogen atmosphere, and calcining for 10 hours at 1600 ℃. The respective raw materials were identical to those used in example 5.
The composite negative electrode materials obtained in the examples and the comparative examples are prepared according to a conventional methodThe negative pole piece and the metal lithium piece are adopted as counter electrodes and adopt 1MLiPF6And+ EC, DEC-1: 1:1 system electrolyte, and a 25-micron thick PE/PP/PE diaphragm of the lithium ion battery to prepare a half battery. The test results are shown in table 1.
The composite negative electrode materials obtained in the examples and comparative examples were used to prepare negative electrodes, LiCoO2As the positive electrode, 1MLiPF is used6And+ EC, DEC-1: 1:1 system electrolyte, and 25-micron-thick PE/PP/PE diaphragm of the lithium ion battery to prepare the full battery. The first charge and discharge and cycle performance of the full cell were measured, and the results are shown in table 1.
Table 1 electrochemical performance test results of half-cell full cells of assembled lithium ion batteries
As can be seen from Table 1, the lithium ion battery half-cells assembled by the composite negative electrode materials obtained in examples 1-5 have higher first discharge gram capacity than comparative examples 1-2, have better rate performance under large current than the comparative examples, and have discharge capacities of 2C, 5C and 6C which are more than 98% of 1C discharge capacity; in addition, the capacity retention rate at 1C rate for 500 cycles of charge and discharge was larger than that of the comparative example. Experimental results show that the composite negative electrode material prepared by treating the graphite tailings by chloroplatinic acid and diethylenetriamine can be used as a novel composite negative electrode material to be applied to the field of lithium ion batteries, and has excellent electrochemical performance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. The composite negative electrode material is characterized by comprising the following raw materials in parts by weight: 31-39 parts of graphite tailings, 3-7 parts of yttrium nitrate, 13-21 parts of chloroplatinic acid, 515-12 parts of epoxy resin E, 3-7 parts of diethylenetriamine, 10-20 parts of graphite and a proper amount of deionized water.
2. The composite anode material of claim 1, wherein the raw materials in parts by weight comprise: 33-37 parts of graphite tailings, 4-6 parts of yttrium nitrate, 15-19 parts of chloroplatinic acid, 517-10 parts of epoxy resin E, 4-6 parts of diethylenetriamine and 12-18 parts of graphite.
3. The composite anode material of claim 1, wherein the raw materials in parts by weight comprise: 35 parts of graphite tailings, 5 parts of yttrium nitrate, 17 parts of chloroplatinic acid, 518 parts of epoxy resin E, 5 parts of diethylenetriamine and 15 parts of graphite.
4. A method for preparing a composite anode material according to any one of claims 1 to 3, comprising the steps of:
1) mixing chloroplatinic acid with deionized water with the mass of 7.5-8 times of that of the chloroplatinic acid to prepare a chloroplatinic acid solution; mixing diethylenetriamine with deionized water in an amount of 4.5 to 5 times the mass of the diethylenetriamine to prepare a diethylenetriamine solution;
2) mixing and grinding the graphite tailings and yttrium nitrate, sieving the mixture through a sieve with the temperature of 100-150 meshes, then mixing the mixture with a chloroplatinic acid solution, heating to the temperature of 58-60 ℃, stirring for 50-60min at the temperature, heating to the temperature of 120-125 ℃, and sealing and stirring for 25-30min at the temperature; then adding diethylenetriamine solution, stirring for 1.5-1.8h at the temperature of 80-82 ℃, and then performing suction filtration, washing and drying to obtain a mixture A;
3) and uniformly mixing the mixture A and graphite, crushing the mixture, sieving the mixture by a sieve with 120-fold sand and 150 meshes, uniformly mixing the mixture A and the epoxy resin E51, calcining the mixture for 5.5 to 6 hours at the temperature of 500 ℃ in a protective atmosphere, and calcining the mixture for 8 to 10 hours at the temperature of 1500-fold sand and 1600 ℃ to obtain the catalyst.
5. The method for preparing the composite anode material according to claim 4, wherein the protective atmosphere is one of helium, nitrogen and argon.
6. The method for preparing the composite anode material as claimed in claim 4, wherein the stirring speed after mixing with the chloroplatinic acid solution in the step 2) is 250-300 r/min.
7. The method for preparing the composite negative electrode material as claimed in claim 4, wherein the stirring speed after the addition of the diethylenetriamine solution in the step 2) is 180-200 r/min.
8. Use of a composite anode material according to any of claims 1 to 3 in a battery.
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|---|---|---|---|---|
| CN1215416A (en) * | 1996-05-08 | 1999-04-28 | 大曹株式会社 | Crss-linked solid polyelectrolyte and use thereof |
| CN103022446A (en) * | 2012-12-19 | 2013-04-03 | 深圳市贝特瑞新能源材料股份有限公司 | Silicon oxide/carbon cathode material of lithium ion battery and preparation method of material |
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