CN107863527A - A kind of composite negative pole material and its preparation method and application - Google Patents
A kind of composite negative pole material and its preparation method and application Download PDFInfo
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- CN107863527A CN107863527A CN201710927689.6A CN201710927689A CN107863527A CN 107863527 A CN107863527 A CN 107863527A CN 201710927689 A CN201710927689 A CN 201710927689A CN 107863527 A CN107863527 A CN 107863527A
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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
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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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- 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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- Battery Electrode And Active Subsutance (AREA)
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Abstract
The invention discloses a kind of composite negative pole material and its preparation method and application, the composite negative pole material, includes according to the raw material of parts by weight:31 39 parts of graphite tailing, 37 parts of yttrium nitrate, 13 21 parts of chloroplatinic acid, 5 12 parts of epoxy resin E51,37 parts of diethylenetriamines, 10 20 parts of graphite.Stirred by graphite tailing, yttrium nitrate mixed grinding, with platinum acid chloride solution Hybrid Heating;Then add diethylenetriamines solution heating stirring, then through filtering, wash, dry after be well mixed and crush with graphite again, then mixed with epoxy resin E51, calcine and produce.Negative material produced by the present invention has good chemical property, can improve reversible specific capacity, efficiency for charge-discharge, stable cycle performance and the high rate performance of lithium ion battery;Graphite tailing can also be reused, and effect is extremely notable, and preparation technology is simple, is adapted to large-scale industrial production.
Description
Technical field
The present invention relates to cell art, specifically a kind of composite negative pole material and its preparation method and application.
Background technology
Compared with traditional plumbic acid, NI-G secondary cell, lithium ion battery have operating voltage it is high, it is higher than energy, work
The advantages that temperature range is wide, electric discharge is steady, have extended cycle life, memory-less effect, therefore it is wide as a kind of novel energy-storing power supply
It is general to be applied to the fields such as communication equipment, electric tool, Aero-Space.
With the continuous progress of technology, people propose higher requirement to lithium ion battery, have high-energy-density, height
The lithium ion battery of the performances such as high rate performance, long circulation life, high safety factor is increasingly becoming the study hotspot of people.Stone at present
Ink is the carbon negative electrode material of lithium ion cell of main commercialization.Graphene is also increasingly paid attention to, but graphite, graphene valency
Lattice are expensive, using limited.And graphite tailing cost is low, takes a large amount of earth's surfaces, destroyed soil, also easily occur landslide,
Mud-rock flow accident, but the effect of graphite tailing in the battery is too poor, can not be directly using, it is necessary to handle it.
The content of the invention
It is an object of the invention to provide a kind of composite negative pole material and its preparation method and application, to solve above-mentioned background
The problem of being proposed in technology.
To achieve the above object, the present invention provides following technical scheme:
A kind of composite negative pole material, include according to the raw material of parts by weight:Graphite tailing 31-39 parts, yttrium nitrate 3-7 parts, chlorine
Platinic acid 13-21 parts, epoxy resin E51 5-12 parts, diethylenetriamines 3-7 parts, graphite 10-20 parts.
As the further scheme of the present invention:The composite negative pole material, include according to the raw material of parts by weight:Graphite tailing
33-37 parts, yttrium nitrate 4-6 parts, chloroplatinic acid 15-19 parts, epoxy resin E51 7-10 parts, diethylenetriamines 4-6 parts, graphite
12-18 parts.
As the further scheme of the present invention:The composite negative pole material, include according to the raw material of parts by weight:Graphite tailing
35 parts, 5 parts of yttrium nitrate, 17 parts of chloroplatinic acid, 8 parts of epoxy resin E51,5 parts of diethylenetriamines, 15 parts of graphite.
A kind of preparation method of composite negative pole material, comprises the following steps:
1) deionized water of 7.5-8 times of chloroplatinic acid and its quality is mixed, platinum acid chloride solution is made;By diethylenetriamines
Mixed with 4.5-5 times of deionized water of its quality, diethylenetriamines solution is made;
2) by graphite tailing, excessively yttrium nitrate mixed grinding, 100-150 mesh sieves, then mix, be warming up to platinum acid chloride solution
58-60 DEG C and stir process 50-60min at such a temperature, then heat to 120-125 DEG C and seal at such a temperature at stirring
Manage 25-30min;Then diethylenetriamines solution, and the stir process 1.5-1.8h at a temperature of 80-82 DEG C are added, then is passed through
Filter, wash, drying obtained mixture A;
3) mixture A is well mixed with graphite and crushed 120-150 mesh sieves, then mixed with epoxy resin E51
It is even, 5.5-6h then is calcined in protective atmosphere, at a temperature of 500 DEG C, then calcines 8- at a temperature of 1500-1600 DEG C again
10h is produced.
As the further scheme of the present invention:Protective atmosphere is using one kind in helium, nitrogen, argon gas.
As the further scheme of the present invention:It is 250- with the mixed mixing speed of platinum acid chloride solution in step 2)
300r/min。
As the further scheme of the present invention:In step 2), the mixing speed added after diethylenetriamines solution is
180-200r/min。
Another object of the present invention is to provide the application of the composite negative pole material in the battery.
Compared with prior art, the beneficial effects of the invention are as follows:
The present invention is handled graphite tailing using chloroplatinic acid, diethylenetriamines, then by made from other techniques
Negative material has good chemical property, can improve the reversible specific capacity, efficiency for charge-discharge, cycle performance of lithium ion battery
Stable and high rate performance;Graphite tailing can also be reused, and effect is extremely notable, and preparation technology is simple, easy to operate,
Raw material sources are extensive, and cost is low, are adapted to large-scale industrial production.Lithium ion can be applied to as a kind of new negative material
Field of batteries, and there is excellent chemical property.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of composite negative pole material, including following raw material:Graphite tailing 31kg, yttrium nitrate 3kg,
Chloroplatinic acid 13kg, epoxy resin E51 5kg, diethylenetriamines 3kg, graphite 10kg.
7.5 times of deionized water of chloroplatinic acid and its quality is mixed, platinum acid chloride solution is made;By diethylenetriamines and its
The deionized water mixing that 4.5 times of quality, is made diethylenetriamines solution.By graphite tailing, yttrium nitrate mixed grinding, cross 100
Mesh sieve, then mixed with platinum acid chloride solution, be warming up to 58 DEG C and at such a temperature stir process 50min, then heat to 120 DEG C
And stir process 25min is sealed at such a temperature;It is 250r/min wherein with the mixed mixing speed of platinum acid chloride solution.Then
Diethylenetriamines solution, and the stir process 1.5h at a temperature of 80 DEG C are added, then through filtering, washing, dry obtained mixing
Thing A;The mixing speed added after diethylenetriamines solution is 180r/min.Mixture A is well mixed and crushed with graphite
120 mesh sieves are crossed, then are well mixed with epoxy resin E51, then calcine 5.5h in helium atmosphere, at a temperature of 500 DEG C, then
Again 8h is calcined at a temperature of 1500 DEG C to produce.
Embodiment 2
In the embodiment of the present invention, a kind of composite negative pole material, including following raw material:Graphite tailing 39kg, yttrium nitrate 7kg,
Chloroplatinic acid 21kg, epoxy resin E51 12kg, diethylenetriamines 7kg, graphite 20kg.
8 times of deionized water of chloroplatinic acid and its quality is mixed, platinum acid chloride solution is made;By diethylenetriamines and its matter
The deionized water mixing of 5 times of amount, is made diethylenetriamines solution.By graphite tailing, yttrium nitrate mixed grinding, 150 mesh sieves are crossed,
Then mixed with platinum acid chloride solution, be warming up to 60 DEG C and at such a temperature stir process 60min, then heat to 125 DEG C and
Stir process 30min is sealed at this temperature;It is 300r/min wherein with the mixed mixing speed of platinum acid chloride solution.Then add
Diethylenetriamines solution, and the stir process 1.8h at a temperature of 82 DEG C, then through filtering, washing, dry obtained mixture A;
The mixing speed added after diethylenetriamines solution is 200r/min.Mixture A is well mixed and crushed with graphite
150 mesh sieves, then be well mixed with epoxy resin E51,6h then is calcined in argon gas atmosphere, at a temperature of 500 DEG C, is then existed again
10h is calcined at a temperature of 1600 DEG C to produce.
Embodiment 3
In the embodiment of the present invention, a kind of composite negative pole material, including following raw material:Graphite tailing 33kg, yttrium nitrate 4kg,
Chloroplatinic acid 15kg, epoxy resin E51 7kg, diethylenetriamines 4kg, graphite 12kg.
8 times of deionized water of chloroplatinic acid and its quality is mixed, platinum acid chloride solution is made;By diethylenetriamines and its matter
The deionized water mixing of 5 times of amount, is made diethylenetriamines solution.By graphite tailing, yttrium nitrate mixed grinding, 120 mesh sieves are crossed,
Then mixed with platinum acid chloride solution, be warming up to 59 DEG C and at such a temperature stir process 55min, then heat to 122 DEG C and
Stir process 30min is sealed at this temperature;It is 280r/min wherein with the mixed mixing speed of platinum acid chloride solution.Then add
Diethylenetriamines solution, and the stir process 1.8h at a temperature of 81 DEG C, then through filtering, washing, dry obtained mixture A;
The mixing speed added after diethylenetriamines solution is 200r/min.Mixture A is well mixed and crushed with graphite
150 mesh sieves, then be well mixed with epoxy resin E51,6h then is calcined in nitrogen atmosphere, at a temperature of 500 DEG C, is then existed again
10h is calcined at a temperature of 1600 DEG C to produce.
Embodiment 4
In the embodiment of the present invention, a kind of composite negative pole material, including following raw material:Graphite tailing 37kg, yttrium nitrate 6kg,
Chloroplatinic acid 19kg, epoxy resin E51 10kg, diethylenetriamines 6kg, graphite 18kg.
8 times of deionized water of chloroplatinic acid and its quality is mixed, platinum acid chloride solution is made;By diethylenetriamines and its matter
The deionized water mixing of 5 times of amount, is made diethylenetriamines solution.By graphite tailing, yttrium nitrate mixed grinding, 120 mesh sieves are crossed,
Then mixed with platinum acid chloride solution, be warming up to 59 DEG C and at such a temperature stir process 55min, then heat to 122 DEG C and
Stir process 30min is sealed at this temperature;It is 280r/min wherein with the mixed mixing speed of platinum acid chloride solution.Then add
Diethylenetriamines solution, and the stir process 1.8h at a temperature of 81 DEG C, then through filtering, washing, dry obtained mixture A;
The mixing speed added after diethylenetriamines solution is 200r/min.Mixture A is well mixed and crushed with graphite
150 mesh sieves, then be well mixed with epoxy resin E51,6h then is calcined in nitrogen atmosphere, at a temperature of 500 DEG C, is then existed again
10h is calcined at a temperature of 1600 DEG C to produce.
Embodiment 5
In the embodiment of the present invention, a kind of composite negative pole material, including following raw material:Graphite tailing 35kg, yttrium nitrate 5kg,
Chloroplatinic acid 17kg, epoxy resin E51 8kg, diethylenetriamines 5kg, graphite 15kg.
8 times of deionized water of chloroplatinic acid and its quality is mixed, platinum acid chloride solution is made;By diethylenetriamines and its matter
The deionized water mixing of 5 times of amount, is made diethylenetriamines solution.By graphite tailing, yttrium nitrate mixed grinding, 120 mesh sieves are crossed,
Then mixed with platinum acid chloride solution, be warming up to 59 DEG C and at such a temperature stir process 55min, then heat to 122 DEG C and
Stir process 30min is sealed at this temperature;It is 280r/min wherein with the mixed mixing speed of platinum acid chloride solution.Then add
Diethylenetriamines solution, and the stir process 1.8h at a temperature of 81 DEG C, then through filtering, washing, dry obtained mixture A;
The mixing speed added after diethylenetriamines solution is 200r/min.Mixture A is well mixed and crushed with graphite
150 mesh sieves, then be well mixed with epoxy resin E51,6h then is calcined in nitrogen atmosphere, at a temperature of 500 DEG C, is then existed again
10h is calcined at a temperature of 1600 DEG C to produce.
Comparative example 1
In addition to chloroplatinic acid, diethylenetriamines is not contained, remaining raw material is consistent with embodiment 5 with technique.
Comparative example 2
Graphite tailing, yttrium nitrate, chloroplatinic acid, diethylenetriamines are directly mixed, addition deionized water be (deionized water
Addition is consistent with embodiment 5), the stir process 1.8h at a temperature of 81 DEG C, then through filtering, washing, dry obtained mixture
A;Mixing speed is 200r/min.Mixture A is well mixed with graphite and crushed 150 mesh sieves, then with epoxy resin E51
It is well mixed, then in nitrogen atmosphere, 6h is calcined at a temperature of 500 DEG C, then calcining 10h at a temperature of 1600 DEG C again is
.Its each raw material is consistent with the raw material and component that are used in embodiment 5.
Cathode pole piece is conventionally made in composite negative pole material obtained by embodiment and comparative example, metal lithium sheet is opposed
Electrode, using 1MLiPF6+EC:EMC:DEC=1:1:1 system electrolyte, 25 μ m-thick lithium ion battery PE/PP/PE barrier films, system
Standby half-cell.Test result is as shown in table 1.
Negative pole, LiCoO is made in composite negative pole material obtained by the present embodiment and comparative example2Make positive pole, using 1MLiPF6+
EC:EMC:DEC=1:1:1 system electrolyte, 25 μ m-thick lithium ion battery PE/PP/PE barrier films, prepares full battery.To the full electricity
The first charge-discharge and cycle performance in pond are detected, as a result as shown in table 1.
The chemical property testing result for the full battery of lithium ion battery half-cell that table 1 assembles
As it can be seen from table 1 the head using the lithium ion battery half-cell of composite negative pole material assembling obtained by embodiment 1-5
Secondary electric discharge gram volume is above comparative example 1-2, and the high rate performance under high current is outstanding compared with comparative example, with 2C, 5C, 6C electric discharge
Capacity is more than the 98% of 1C discharge capacities respectively;In addition, the capability retention of discharge and recharge 500 weeks compares ratio under 1C multiplying powers
The capability retention of example is big.Test result indicates that graphite tailing is handled using chloroplatinic acid, diethylenetriamines and this
Composite negative pole material made from invented technology can be applied to field of lithium ion battery as a kind of new composite negative pole material, and
With excellent chemical property.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
It is appreciated that other embodiment.
Claims (8)
1. a kind of composite negative pole material, it is characterised in that include according to the raw material of parts by weight:Graphite tailing 31-39 parts, yttrium nitrate
3-7 parts, chloroplatinic acid 13-21 parts, epoxy resin E51 5-12 parts, diethylenetriamines 3-7 parts, graphite 10-20 parts.
2. composite negative pole material according to claim 1, it is characterised in that include according to the raw material of parts by weight:Graphite tail
Ore deposit 33-37 parts, yttrium nitrate 4-6 parts, chloroplatinic acid 15-19 parts, epoxy resin E51 7-10 parts, diethylenetriamines 4-6 parts, graphite
12-18 parts.
3. composite negative pole material according to claim 1, it is characterised in that include according to the raw material of parts by weight:Graphite tail
35 parts of ore deposit, 5 parts of yttrium nitrate, 17 parts of chloroplatinic acid, 8 parts of epoxy resin E51,5 parts of diethylenetriamines, 15 parts of graphite.
4. the preparation method of a kind of composite negative pole material as described in claim 1-3 is any, it is characterised in that including following step
Suddenly:
1)7.5-8 times of deionized water of chloroplatinic acid and its quality is mixed, platinum acid chloride solution is made;By diethylenetriamines and its
The deionized water mixing of 4.5-5 times of quality, is made diethylenetriamines solution;
2)By graphite tailing, yttrium nitrate mixed grinding, 100-150 mesh sieves are crossed, is then mixed with platinum acid chloride solution, is warming up to 58-
60 DEG C and stir process 50-60min at such a temperature, then heat to 120-125 DEG C and seal stir process at such a temperature
25-30min;Then diethylenetriamines solution, and the stir process 1.5-1.8h at a temperature of 80-82 DEG C are added, then through taking out
Filter, washing, dry obtained mixture A;
3)Mixture A is well mixed with graphite and crushed 120-150 mesh sieves, then is well mixed with epoxy resin E51, so
Afterwards in protective atmosphere, 5.5-6h is calcined at a temperature of 500 DEG C, then again at a temperature of 1500-1600 DEG C calcine 8-10h be
.
5. the preparation method of composite negative pole material according to claim 4, it is characterised in that protective atmosphere using helium,
One kind in nitrogen, argon gas.
6. the preparation method of composite negative pole material according to claim 4, it is characterised in that step 2)In, with chloroplatinic acid
The mixed mixing speed of solution is 250-300r/min.
7. the preparation method of composite negative pole material according to claim 4, it is characterised in that step 2)In, it is sub- to add two
Mixing speed after ethyl triamine solution is 180-200r/min.
8. the application of composite negative pole material in the battery as described in claim 1-3 is any.
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