CN106169605A - A kind of modified polyaniline positive electrode and preparation method thereof - Google Patents
A kind of modified polyaniline positive electrode and preparation method thereof Download PDFInfo
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- CN106169605A CN106169605A CN201610687476.6A CN201610687476A CN106169605A CN 106169605 A CN106169605 A CN 106169605A CN 201610687476 A CN201610687476 A CN 201610687476A CN 106169605 A CN106169605 A CN 106169605A
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
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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
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
- H01M4/602—Polymers
- H01M4/606—Polymers containing aromatic main chain polymers
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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
Abstract
The invention discloses a kind of modified polyaniline positive electrode and preparation method thereof, described modified polyaniline positive electrode, according to the primary raw material of weight portion be: modified polyaniline 35 45 parts, lithium acetate 12 18 parts, tetraethyl orthosilicate 8 10 parts, polysulfideization slowly acid 26 parts, Barium metatitanate. 26 parts, nanometer sodium carboxymethyl cellulose 0.3 1.4 parts；The preparation method of described modified polyaniline is: mixed with pyrroles, ceramic particle, manganese chloride, glass fibre by polyaniline, calcines 1h, be vacuum dried and get final product at 1245 DEG C.Prepared lithium ion battery has the cycle performance of excellence, and under room temperature, 2000 capacity of 1C charge and discharge circulation are maintained at more than 90%；Under 6C multiplying power, electric discharge is more than the 98% of 1C capacity；3C/10V overcharges test, and battery is the most on fire does not explodes；High temperature circulation is excellent, and at 60 DEG C, 1000 capacity of 1C charge and discharge circulation are maintained at more than 88%；There is good security performance, acupuncture, extrude, overcharge, cross put etc. test do not explode, the most on fire.
Description
Technical field
The present invention relates to a kind of lithium electro-technical field, specifically a kind of modified polyaniline positive electrode and preparation method thereof.
Background technology
Lithium ion battery has that running voltage is high, specific energy high, has extended cycle life, electric discharge lightweight, white less, memoryless effect
Should be with cost performance advantages of higher, it has also become high power electric vehicle, artificial satellite, the master of Aero-Space lamp field rechargeable type power supply
Object to be selected.It addition, the system of positive and negative pole material composition has a common feature to discharge the later stage exactly, especially at electric discharge knot
Shu Shi, voltage declines very fast, namely inside this voltage range, the capacity of lithium ion battery almost without.
Summary of the invention
It is an object of the invention to provide a kind of modified polyaniline positive electrode and preparation method thereof, to solve above-mentioned background
The problem proposed in technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of modified polyaniline positive electrode, according to the primary raw material of weight portion be: modified polyaniline 35-45 part, acetic acid
Lithium 12-18 part, tetraethyl orthosilicate 8-10 part, polysulfideization slowly acid 2-6 part, Barium metatitanate. 2-6 part, nanometer sodium carboxymethyl cellulose 0.3-
1.4 part；The preparation method of described modified polyaniline is: mixed with pyrroles, ceramic particle, manganese chloride, glass fibre by polyaniline,
Calcine 1h at 1245 DEG C, be vacuum dried and get final product.
As the further scheme of the present invention: described modified polyaniline positive electrode, according to the primary raw material of weight portion it is:
Modified polyaniline 39-42 part, lithium acetate 14-17 part, tetraethyl orthosilicate 8-10 part, polysulfideization slowly acid 2-6 part, Barium metatitanate. 2-6 part,
Nanometer sodium carboxymethyl cellulose 0.8-1.1 part；The preparation method of described modified polyaniline is: by polyaniline and pyrroles, pottery
Grain, manganese chloride, glass fibre mix, and calcine 1h, be vacuum dried and get final product at 1245 DEG C.
As the further scheme of the present invention: described modified polyaniline positive electrode, according to the primary raw material of weight portion it is:
The slowly acid 4 parts of modified polyaniline 40 parts, lithium acetate 16 parts, tetraethyl orthosilicate 9 parts, polysulfideization, Barium metatitanate. 5 parts, nanometer carboxymethyl fibre
Dimension 0.9 part of sodium of element；The preparation method of described modified polyaniline is: by polyaniline and pyrroles, ceramic particle, manganese chloride, glass fibers
Dimension mixing, calcines 1h, is vacuum dried and get final product at 1245 DEG C.
As the further scheme of the present invention: the purity of described polyaniline is more than 99.9%.
As the further scheme of the present invention: the mesh number of described Barium metatitanate. is 1200 mesh.
As the further scheme of the present invention: the mesh number of described ceramic particle is 1200 mesh.
The preparation method of a kind of modified polyaniline positive electrode, concretely comprises the following steps:
(1) first, modified polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 700 DEG C-800 DEG C also
Stirring 60min-90min, makes semi-finished product；
(2) last, semi-finished product are carried out with tetraethyl orthosilicate, polysulfideization slowly acid, Barium metatitanate., nanometer sodium carboxymethyl cellulose
Mixing stirring, speed of agitator is 400r/min, and mixing time is 45min, carries out roasting in 1200 DEG C subsequently, and vacuum drying is i.e.
?.
As the further scheme of the present invention: step (1) is heated to 750 DEG C and stirs 82min.
Compared with prior art, the invention has the beneficial effects as follows:
Prepared lithium ion battery has the cycle performance of excellence, and under room temperature, 2000 capacity of 1C charge and discharge circulation are maintained at
More than 90%；Under 6C multiplying power, electric discharge is more than the 98% of 1C capacity；3C/10V overcharges test, and battery is the most on fire does not explodes；High temperature follows
Ring is excellent, and at 60 DEG C, 1000 capacity of 1C charge and discharge circulation are maintained at more than 88%；There is good security performance, acupuncture, extruding,
Overcharge, cross put etc. test do not explode, the most on fire.
Detailed description of the invention
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 a part of 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 not making creative work premise, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of modified polyaniline positive electrode, according to the primary raw material of weight portion be: modified polyaniline 35 parts, lithium acetate 12
Part, tetraethyl orthosilicate 8 parts, polysulfideization slowly acid 2 parts, Barium metatitanate. 2 parts, nanometer sodium carboxymethyl cellulose 0.3 part；Described modified polyphenyl
The preparation method of amine is: mixed with pyrroles, ceramic particle, manganese chloride, glass fibre by polyaniline, calcines 1h, very at 1245 DEG C
Sky is drying to obtain；The purity of described polyaniline is more than 99.9%；The mesh number of described Barium metatitanate. is 1200 mesh；Described ceramic particle
Mesh number be 1200 mesh.
The preparation method of a kind of modified polyaniline positive electrode, concretely comprises the following steps:
(1) first, modified polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 700 DEG C and stirs
60min, makes semi-finished product；
(2) last, semi-finished product are carried out with tetraethyl orthosilicate, polysulfideization slowly acid, Barium metatitanate., nanometer sodium carboxymethyl cellulose
Mixing stirring, speed of agitator is 400r/min, and mixing time is 45min, carries out roasting in 1200 DEG C subsequently, and vacuum drying is i.e.
?.
Embodiment 2
A kind of modified polyaniline positive electrode, according to the primary raw material of weight portion be: modified polyaniline 39 parts, lithium acetate 14
Part, tetraethyl orthosilicate 8 parts, polysulfideization slowly acid 2 parts, Barium metatitanate. 2 parts, nanometer sodium carboxymethyl cellulose 0.8 part；Described modified polyphenyl
The preparation method of amine is: mixed with pyrroles, ceramic particle, manganese chloride, glass fibre by polyaniline, calcines 1h, very at 1245 DEG C
Sky is drying to obtain；The purity of described polyaniline is more than 99.9%；The mesh number of described Barium metatitanate. is 1200 mesh；Described ceramic particle
Mesh number be 1200 mesh.
The preparation method of a kind of modified polyaniline positive electrode, concretely comprises the following steps:
(1) first, modified polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 700 DEG C and stirs
60min, makes semi-finished product；
(2) last, semi-finished product are carried out with tetraethyl orthosilicate, polysulfideization slowly acid, Barium metatitanate., nanometer sodium carboxymethyl cellulose
Mixing stirring, speed of agitator is 400r/min, and mixing time is 45min, carries out roasting in 1200 DEG C subsequently, and vacuum drying is i.e.
?.
Embodiment 3
A kind of modified polyaniline positive electrode, according to the primary raw material of weight portion be: modified polyaniline 40 parts, lithium acetate 16
Part, tetraethyl orthosilicate 9 parts, polysulfideization slowly acid 4 parts, Barium metatitanate. 5 parts, nanometer sodium carboxymethyl cellulose 0.9 part；Described modified polyphenyl
The preparation method of amine is: mixed with pyrroles, ceramic particle, manganese chloride, glass fibre by polyaniline, calcines 1h, very at 1245 DEG C
Sky is drying to obtain；The purity of described polyaniline is more than 99.9%；The mesh number of described Barium metatitanate. is 1200 mesh；Described ceramic particle
Mesh number be 1200 mesh.
The preparation method of a kind of modified polyaniline positive electrode, concretely comprises the following steps:
(1) first, modified polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 750 DEG C and stirs
82min, makes semi-finished product；
(2) last, semi-finished product are carried out with tetraethyl orthosilicate, polysulfideization slowly acid, Barium metatitanate., nanometer sodium carboxymethyl cellulose
Mixing stirring, speed of agitator is 400r/min, and mixing time is 45min, carries out roasting in 1200 DEG C subsequently, and vacuum drying is i.e.
?.
Embodiment 4
A kind of modified polyaniline positive electrode, according to the primary raw material of weight portion be: modified polyaniline 42 parts, lithium acetate 17
Part, tetraethyl orthosilicate 10 parts, polysulfideization slowly acid 6 parts, Barium metatitanate. 6 parts, nanometer sodium carboxymethyl cellulose 1.1 parts；Described modification gathers
The preparation method of aniline is: mixed with pyrroles, ceramic particle, manganese chloride, glass fibre by polyaniline, calcines 1h at 1245 DEG C,
It is vacuum dried and get final product；The purity of described polyaniline is more than 99.9%；The mesh number of described Barium metatitanate. is 1200 mesh；Described pottery
The mesh number of grain is 1200 mesh.
The preparation method of a kind of modified polyaniline positive electrode, concretely comprises the following steps:
(1) first, modified polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 800 DEG C and stirs
90min, makes semi-finished product；
(2) last, semi-finished product are carried out with tetraethyl orthosilicate, polysulfideization slowly acid, Barium metatitanate., nanometer sodium carboxymethyl cellulose
Mixing stirring, speed of agitator is 400r/min, and mixing time is 45min, carries out roasting in 1200 DEG C subsequently, and vacuum drying is i.e.
?.
Embodiment 5
A kind of modified polyaniline positive electrode, according to the primary raw material of weight portion be: modified polyaniline 45 parts, lithium acetate 18
Part, tetraethyl orthosilicate 10 parts, polysulfideization slowly acid 6 parts, Barium metatitanate. 6 parts, nanometer sodium carboxymethyl cellulose 1.4 parts；Described modification gathers
The preparation method of aniline is: mixed with pyrroles, ceramic particle, manganese chloride, glass fibre by polyaniline, calcines 1h at 1245 DEG C,
It is vacuum dried and get final product；The purity of described polyaniline is more than 99.9%；The mesh number of described Barium metatitanate. is 1200 mesh；Described pottery
The mesh number of grain is 1200 mesh.
The preparation method of a kind of modified polyaniline positive electrode, concretely comprises the following steps:
(1) first, modified polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 800 DEG C and stirs
90min, makes semi-finished product；
(2) last, semi-finished product are carried out with tetraethyl orthosilicate, polysulfideization slowly acid, Barium metatitanate., nanometer sodium carboxymethyl cellulose
Mixing stirring, speed of agitator is 400r/min, and mixing time is 45min, carries out roasting in 1200 DEG C subsequently, and vacuum drying is i.e.
?.
Comparative example 1
A kind of polyaniline positive electrode, according to the primary raw material of weight portion be: polyaniline 40 parts, lithium acetate 16 parts, positive silicon
Acetoacetic ester 9 parts, Barium metatitanate. 5 parts, nanometer sodium carboxymethyl cellulose 0.9 part；The purity of described polyaniline is more than 99.9%；Described
The mesh number of Barium metatitanate. is 1200 mesh.
The preparation method of a kind of polyaniline positive electrode, concretely comprises the following steps:
(1) first, polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 750 DEG C and stirs 82min,
Make semi-finished product；
(2) last, semi-finished product and tetraethyl orthosilicate, Barium metatitanate., nanometer sodium carboxymethyl cellulose are carried out mixing stirring, stirs
Mixing rotating speed is 400r/min, and mixing time is 45min, carries out roasting in 1200 DEG C subsequently, is drying to obtain.
Comparative example 2
A kind of polyaniline positive electrode, according to the primary raw material of weight portion be: polyaniline 40 parts, lithium acetate 16 parts, positive silicon
Acetoacetic ester 9 parts；The purity of described polyaniline is more than 99.9%.
The preparation method of a kind of polyaniline positive electrode, concretely comprises the following steps:
(1) first, polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 750 DEG C and stirs 82min,
Make semi-finished product；
(2) last, semi-finished product and tetraethyl orthosilicate are carried out mixing stirring, speed of agitator is 400r/min, mixing time
For 45min, carry out roasting in 1200 DEG C subsequently, be drying to obtain.
Comparative example 3
A kind of modified polyaniline positive electrode, according to the primary raw material of weight portion be: modified polyaniline 40 parts, lithium acetate 16
Part, tetraethyl orthosilicate 9 parts, Barium metatitanate. 5 parts, nanometer sodium carboxymethyl cellulose 0.9 part；The preparation method of described modified polyaniline
For: polyaniline is mixed with pyrroles, ceramic particle, manganese chloride, glass fibre, calcines 1h at 1245 DEG C, be vacuum dried and get final product；Institute
The purity stating polyaniline is more than 99.9%；The mesh number of described Barium metatitanate. is 1200 mesh；The mesh number of described ceramic particle is 1200
Mesh.
The preparation method of a kind of modified polyaniline positive electrode, concretely comprises the following steps:
(1) first, modified polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 750 DEG C and stirs
82min, makes semi-finished product；
(2) last, semi-finished product and tetraethyl orthosilicate, Barium metatitanate., nanometer sodium carboxymethyl cellulose are carried out mixing stirring, stirs
Mixing rotating speed is 400r/min, and mixing time is 45min, carries out roasting in 1200 DEG C subsequently, is drying to obtain.
Test experience
Positive electrode prepared by embodiment 1-5 and comparative example 1-3 is prepared as 1665132 model lithium-ion-power cells
(the lamination soft-package battery of model H16*W65*L132mm), compacted density is at 3.0g/cm3Above, volume energy density exists
More than 450Wh/L；Battery core is under 3.0V-4.2V voltage, and 1C electric discharge gram volume plays more than 120mAh/g.
Prepared lithium ion battery has the cycle performance of excellence, and under room temperature, 2000 capacity of 1C charge and discharge circulation are maintained at
More than 90%；Under 6C multiplying power, electric discharge is more than the 98% of 1C capacity；3C/10V overcharges test, and battery is the most on fire does not explodes；High temperature follows
Ring is excellent, and at 60 DEG C, 1000 capacity of 1C charge and discharge circulation are maintained at more than 88%；There is good security performance, acupuncture, extruding,
Overcharge, cross put etc. test do not explode, the most on fire.Concrete test result is shown in Table 1:
Table 1
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 the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter
From the point of view of which point, all should regard embodiment 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 by fall in the implication of equivalency and scope of claim
Change is included in the present invention.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only wraps
Containing an independent technical scheme, this narrating mode of description is only that for clarity sake those skilled in the art should
Description can also be formed those skilled in the art through appropriately combined as an entirety, the technical scheme in each embodiment
May be appreciated other embodiments.
Claims (8)
1. a modified polyaniline positive electrode, it is characterised in that according to the primary raw material of weight portion be: modified polyaniline 35-
45 parts, lithium acetate 12-18 part, tetraethyl orthosilicate 8-10 part, polysulfideization slowly acid 2-6 part, Barium metatitanate. 2-6 part, nanometer carboxymethyl fine
Dimension element sodium 0.3-1.4 part；The preparation method of described modified polyaniline is: by polyaniline and pyrroles, ceramic particle, manganese chloride, glass
Glass fiber mixes, and calcines 1h, be vacuum dried and get final product at 1245 DEG C.
Modified polyaniline positive electrode the most according to claim 1, it is characterised in that described modified polyaniline positive pole material
Material, according to the primary raw material of weight portion be: modified polyaniline 39-42 part, lithium acetate 14-17 part, tetraethyl orthosilicate 8-10 part, poly-
Sulfuration slowly acid 2-6 part, Barium metatitanate. 2-6 part, nanometer sodium carboxymethyl cellulose 0.8-1.1 part；The preparation side of described modified polyaniline
Method is: mixed with pyrroles, ceramic particle, manganese chloride, glass fibre by polyaniline, calcines 1h, be vacuum dried and get final product at 1245 DEG C.
Modified polyaniline positive electrode the most according to claim 1 and 2, it is characterised in that described modified polyaniline positive pole
Material, according to the primary raw material of weight portion be: modified polyaniline 40 parts, lithium acetate 16 parts, tetraethyl orthosilicate 9 parts, polysulfideization are slowly
Acid 4 parts, Barium metatitanate. 5 parts, nanometer sodium carboxymethyl cellulose 0.9 part；The preparation method of described modified polyaniline is: by polyaniline with
Pyrroles, ceramic particle, manganese chloride, glass fibre mixing, calcine 1h, be vacuum dried and get final product at 1245 DEG C.
Modified polyaniline positive electrode the most according to claim 3, it is characterised in that the purity of described polyaniline is
More than 99.9%.
Modified polyaniline positive electrode the most according to claim 4, it is characterised in that the mesh number of described Barium metatitanate. is 1200
Mesh.
Modified polyaniline positive electrode the most according to claim 5, it is characterised in that the mesh number of described ceramic particle is
1200 mesh.
7. the preparation method of the modified polyaniline positive electrode as described in claim 1-6 is arbitrary, it is characterised in that concrete
Step is:
(1) first, modified polyaniline is mixed with lithium acetate, the most under nitrogen protection, is heated to 700 DEG C-800 DEG C and stirs
60min-90min, makes semi-finished product；
(2) last, semi-finished product are mixed with tetraethyl orthosilicate, polysulfideization slowly acid, Barium metatitanate., nanometer sodium carboxymethyl cellulose
Stirring, speed of agitator is 400r/min, and mixing time is 45min, carries out roasting in 1200 DEG C subsequently, is vacuum dried and get final product.
The preparation method of modified polyaniline positive electrode the most according to claim 7, it is characterised in that step adds in (1)
Heat is to 750 DEG C and stirs 82min.
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2016
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| JPH10302766A (en) * | 1997-04-22 | 1998-11-13 | Toshiba Battery Co Ltd | Lithium ion secondary battery |
| CN101499538A (en) * | 2008-02-01 | 2009-08-05 | 索尼株式会社 | Non-aqueous electrolyte cell, anode and manufacturing method of the same |
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Application publication date: 20161130 |
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