CN109742397A - A kind of polymer cathode materials for Li-ion battery, preparation method and application - Google Patents
A kind of polymer cathode materials for Li-ion battery, preparation method and application Download PDFInfo
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- CN109742397A CN109742397A CN201910007153.1A CN201910007153A CN109742397A CN 109742397 A CN109742397 A CN 109742397A CN 201910007153 A CN201910007153 A CN 201910007153A CN 109742397 A CN109742397 A CN 109742397A
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- triphenylamine
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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 present invention discloses a kind of polymer cathode materials for Li-ion battery, preparation method and application, belong to field of lithium ion battery, the present invention synthesizes poly-triphenylamine positive electrode by ionic liquid, not only contribute to the recycling of catalyst, it avoids micro catalyst simultaneously to bring into electrode material, damages battery performance.The present invention is substituted using ionic liquid to environment nocuousness, has virose chloroform as poly-triphenylamine synthetic, and ionic liquid is tasteless, non-ignitable, and vapour pressure is extremely low, reduces the problem of environmental pollution generated by volatilization；Ionic liquid can operating temperature range it is wide, have good thermal stability and chemical stability, easily separate, can recycle with other materials；Molysite ionic liquid prepared by the present invention has catalytic polymerization effect for triphenylamine polymerization；It in addition, prepared molysite ionic liquid combined coefficient is high, can be recycled, and there is magnetism, it can Magnetic Isolation.
Description
Technical field
The present invention relates to field of lithium ion battery, more particularly to a kind of polymer cathode materials for Li-ion battery, preparation
Method and application.
Background technique
Lithium ion battery alleviates dependence and increasingly serious ring of the people to fossil fuel as novel stored energy form
Border pressure.And develop one of the research hotspot that high performance electrode material of lithium battery is always electrochemical energy source domain.With tradition
Inorganic positive electrode is compared, and polymers as cathode materials flexibility is good, cheap and easy to get, environmental-friendly, easy to process, designability is strong
Many advantages, such as.
Currently, poly-triphenylamine (Polytriphenylamine, PTPAn) is considered as the polymer anode material of great potential
Material.In recent years, there is the preparation of patent and paper document report about the polymerization and modified composite material of poly-triphenylamine
Method.In terms of patent, such as triphenylamine derivative polymer (CN102751501A) with triphenylamine, thiophene-structure,
(CN1760235) using triphenylamine as raw material, in the presence of catalyst lewis acid, abundant solid-phase grinding obtains poly-triphenylamine and slightly produces
Product.(CN106207182A) it discloses and micro- mesoporous poly-triphenylamine derivative is made by chemical oxidative polymerization.On the other hand,
There are document report poly-triphenylamine and its excellent properties with other electrode material Application of composite.As (battery industry, 2010,15
(03): 165-168. it) reports using triphenylamine as raw material, ferric trichloride is catalyst, has synthesized poly- triphen using chemical method
Amine is tested in organic electrolyte system as anode active material of lithium ion battery.Discharge capacity reaches for the first time
101.34mAh/g and cycle performance is good.(Acta PhySico-Chimica Sinica 2014,30 (1): 88-94) passes through solution blended process,
PTPAn can densely be coated on the surface C-LiFePO4, and material first discharge specific capacity is under 0.1C multiplying power constant current charge-discharge
154.5mAh·g-1, the specific discharge capacity of material reaches 114.2mAhg under 10C high magnification constant current charge-discharge-1。
The aniline unit of poly- (to benzene) structure and high-energy density in the molecular structure of poly-triphenylamine with high conductivity
Structure, compares polyaniline, and poly-triphenylamine has better thermal stability.The main method for the synthesis poly-triphenylamine reported at present
In, it needs to use ferric trichloride for oxidant, chloroform is as solvent.Due to using Solid Ferric Trichloride as catalyst, anti-
Poly-triphenylamine can be made fine and close in its surface aggregation during answering.And it can inhibit in the poly-triphenylamine of ferric trichloride Surface Creation
Further progress is reacted, the poly-triphenylamine being synthesized is also resulted in and contains more ferric trichloride impurity, subsequent processing is cumbersome.Separately
On the one hand, chloroform has very strong volatility, and meeting illumination can act on the oxygen in air, gradually decomposes and generate the phosgene of severe toxicity
(phosgene) and hydrogen chloride have certain toxicity, and harmful to environment, can pollute to water body.
Ionic liquid is a kind of green solvent, has good catalytic action in catalytic hydrogenation, the reaction such as catalysis oxidation.
And magnetic ionic liquids are as a kind of functional form ionic liquid, in Magnetic Isolation, metal catalytic, materials synthesis, mass-and heat-transfer etc.
Aspect even more has huge application potential.
Summary of the invention
The object of the present invention is to provide a kind of polymer cathode materials for Li-ion batteries, preparation method and application, to solve
The above-mentioned problems of the prior art.
To achieve the above object, the present invention provides following schemes:
The present invention provides a kind of preparation method of polymer cathode materials for Li-ion battery, comprising the following steps:
Triphenylamine is added in molysite ionic liquid, stirring 2~48h under inert gas protection reacts it sufficiently；So
Afterwards, solution being placed in methanol and stands 1~7 day, filtered, gained precipitating is washed with methanol, after being stirred overnight in saturation ammonium hydroxide,
Filtering is to get poly-triphenylamine positive electrode.
Further, the synthetic method of the molysite ionic liquid is as follows: ionic liquid is mixed at a temperature of 20~100 DEG C
It closes uniformly, ferric trichloride is added in ionic liquid under inert gas protection, 2~48h of stirring reacts it sufficiently.
Further, the ionic liquid be 1- allyl -3- methylimidazolium chloride, 1- decyl -3- methylimidazole villaumite,
1- octyl -3- methylimidazole villaumite, 1- butyl -2,3- methylimidazole villaumite, 1- ethyl-3-methylimidazole villaumite, 1- hexyl -
Or mixtures thereof one of 3- methylimidazole villaumite, N-Methyl pyrrolidone villaumite, triethylamine hydrochloride.
Further, the molar ratio of the ferric trichloride and ionic liquid is 1~2:1.
Further, the molar ratio of the molysite ionic liquid and triphenylamine is 1~3:1.
The present invention also provides poly- triphens made from a kind of preparation method of above-mentioned polymer cathode materials for Li-ion battery
Amine positive electrode.
The present invention also provides a kind of above-mentioned poly-triphenylamine positive electrodes to prepare the application in poly-triphenylamine anode electrode,
Include the following steps,
(1) preparation of anode sizing agent: as a positive electrode active material by the poly-triphenylamine positive electrode, with conductive agent acetylene
It is black to be thoroughly mixed uniformly, bonding agent PVDF is stirring evenly and then adding into dry-mixed, it is dry-mixed to add N- methyl after mixing evenly
Pyrrolidones forms slurry, controls the solid content and slurry viscosity of slurry, obtains anode sizing agent；
(2) preparation of anode electrode: step (1) described anode sizing agent is coated on aluminium foil, is ground on milling roller
Pressure obtains poly-triphenylamine anode electrode after punching.
Further, the anode sizing agent includes following components in mass ratio, and poly-triphenylamine positive electrode accounts for 50%~
80%, conductive agent acetylene black accounts for 10%~30%, bonding agent PVDF and accounts for 10%~20%.
Further, the solid content in the anode sizing agent is 40~60%, and slurry viscosity is 4500~6000cps.
Molysite ionic liquid can be recycled by following steps and be used in the present invention:
Ionic liquid is quickly separated with most water using Magnetic Isolation means, then is added into molysite ionic liquid
The 4A type molecular sieve of activation, arrest reaction 24 hours with a small amount of moisture in adion liquid, after being removed water after filtering
Molysite ionic liquid, molecular sieve continue to use after can drying.
The invention discloses following technical effects:
The present invention uses molysite ionic-liquid catalyst, synthesizes high-purity poly-triphenylamine, not only contributes to the recycling of catalyst,
It avoids micro catalyst simultaneously to bring into electrode material, damages battery performance.
The present invention is substituted using ionic liquid to environment nocuousness, has virose chloroform as solvent.Ionic liquid is tasteless,
Non-ignitable, vapour pressure is extremely low, reduces the problem of environmental pollution generated by volatilization；Can operating temperature range it is wide by (- 40~300
DEG C), there is good thermal stability and chemical stability, easily separate, can recycle with other materials.
Molysite ionic liquid prepared by the present invention has catalytic polymerization effect for triphenylamine polymerization；In addition, prepared
Molysite ionic liquid combined coefficient it is high, can be recycled, and there is magnetism, can Magnetic Isolation.To solve the prior art
The shortcomings that and shortcoming.
Detailed description of the invention
Fig. 1 is the infared spectrum of 1 poly-triphenylamine positive electrode of embodiment；
Fig. 2 is the charging and discharging curve of 1 button cell of embodiment；
Fig. 3 is the cycle performance figure of 1 button cell of embodiment.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing and specific real
Applying mode, the present invention is described in further detail.
Embodiment 1
By 0.1mol 1- ethyl-3-methylimidazole villaumite, 0.1mol N-Methyl pyrrolidone villaumite and 0.1mol 1-
During hexyl -3- methylimidazole villaumite is uniformly mixed at 80 DEG C, under protection of argon gas by 0.3mol anhydrous ferric trichloride at 80 DEG C
At a temperature of be added in solution, stirring react it sufficiently for 24 hours, obtain molysite ionic liquid.
The triphenylamine (TPAn) of 0.1mol is added in molysite ionic liquid, 70 DEG C of stirrings make it for 24 hours under protection of argon gas
Sufficiently reaction.Precipitating is collected in filtering, is washed three times with methanol, by being deposited in saturation ammonium hydroxide after washing, mistake after being stirred overnight
Filter, obtains poly-triphenylamine positive electrode, infrared spectrum is as shown in Figure 1.
As a positive electrode active material by obtained poly-triphenylamine positive electrode, it is sufficiently mixed with conductive agent acetylene black uniformly,
Poly-triphenylamine account for poly-triphenylamine, acetylene black, PVDF three's gross mass 50%, acetylene black accounts for the 30% of gross mass, dry-mixed
It is stirring evenly and then adding into bonding agent PVDF, PVDF accounts for the 20% of gross mass, dry-mixed to add N- crassitude after mixing evenly
Ketone forms slurry, and the solid content for controlling slurry is 40%, and slurry viscosity 4500cps obtains anode sizing agent.Anode sizing agent is coated with
It on aluminium foil, is rolled on milling roller, poly-triphenylamine electrode is obtained after punching.
Using above-mentioned electrode as anode, lithium metal uses 1.0mol/L LiPF as cathode, electrolyte6- EC+DMC (body
Product is than being 1:1), button cell is assembled into the dry glove box full of argon gas.Shelve it is carried out after 12h cycle performance and
Charge-discharge performance test.First circle charging and discharging curve as shown in Fig. 2, cycle performance test results are shown in figure 3.Conventional method preparation
The discharge capacity for the first time of poly-triphenylamine be about 100mAh g-1, and use its discharge capacity for the first time of the poly-triphenylamine of method preparation
Up to 132.6mAh g-1, 80 circle after discharge capacity be 125.6mAh g-1Even if 80 circle circulation after discharge capacity also much larger than
The initial capacity of conventional method, capacity retention ratio is up to 94.7%.
Molysite ionic liquid in the present embodiment can be recycled by following steps to be used:
Ionic liquid is quickly separated with most water using Magnetic Isolation means, then is added into molysite ionic liquid
The 4A type molecular sieve of activation, arrest reaction 24 hours with a small amount of moisture in adion liquid, after being removed water after filtering
Molysite ionic liquid, molecular sieve continue to use after can drying.
Embodiment 2
By 0.2mol 1- allyl -3- methylimidazolium chloride, 0.2mol 1- decyl -3- methylimidazole villaumite and
0.2mol 1- octyl -3- methylimidazole villaumite is uniformly mixed at 60 DEG C, ionic liquid is obtained, under protection of argon gas by 1.2mol
Anhydrous ferric trichloride is added in solution at a temperature of 60 DEG C, and stirring 48h reacts it sufficiently, obtains molysite ionic liquid.
The triphenylamine (TPAn) of 0.6mol is added in above-mentioned molysite ionic liquid, under protection of argon gas 60 DEG C of stirrings
48h reacts it sufficiently, and precipitating is collected in filtering, washs precipitating three times with methanol, the precipitating after washing is placed in saturation ammonium hydroxide
In, poly-triphenylamine positive electrode is obtained by filtration after being stirred overnight.
As a positive electrode active material by obtained poly-triphenylamine positive electrode, it is sufficiently mixed with conductive agent acetylene black uniformly,
Poly-triphenylamine account for poly-triphenylamine, acetylene black, PVDF three's gross mass 80%, acetylene black accounts for the 10% of gross mass, stirs dry-mixed
Bonding agent PVDF is added after mixing uniformly, PVDF accounts for the 10% of gross mass, dry-mixed to add N-Methyl pyrrolidone after mixing evenly
Slurry is formed, the solid content for controlling slurry is 50%, and slurry viscosity 5000cps obtains anode sizing agent.Anode sizing agent is coated on
It on aluminium foil, is rolled on milling roller, poly-triphenylamine electrode is obtained after punching.
Embodiment 3
0.3mol 1- butyl -2,3- methylimidazole villaumite, 0.3mol triethylamine hydrochloride are uniformly mixed at 100 DEG C,
Ionic liquid is obtained, is under nitrogen protection added to 1.2mol anhydrous ferric trichloride in solution at a temperature of 100 DEG C, is stirred
36h reacts it sufficiently, obtains molysite ionic liquid.
The triphenylamine (TPAn) of 1.2mol is added in above-mentioned molysite ionic liquid, under nitrogen protection 100 DEG C of stirrings
12h reacts it sufficiently, and precipitating is collected in filtering, washs precipitating three times with methanol, the precipitating after washing is placed in saturation ammonium hydroxide
In, poly-triphenylamine positive electrode is obtained by filtration after being stirred overnight.
As a positive electrode active material by obtained poly-triphenylamine positive electrode, it is sufficiently mixed with conductive agent acetylene black uniformly,
Poly-triphenylamine account for poly-triphenylamine, acetylene black, PVDF three's gross mass 70%, acetylene black accounts for the 20% of gross mass, stirs dry-mixed
Bonding agent PVDF is added after mixing uniformly, PVDF accounts for the 10% of gross mass, dry-mixed to add N-Methyl pyrrolidone after mixing evenly
Slurry is formed, the solid content for controlling slurry is 60%, and slurry viscosity 6000cps obtains anode sizing agent.Anode sizing agent is coated on
It on aluminium foil, is rolled on milling roller, poly-triphenylamine electrode is obtained after punching.
Embodiment 4
0.6mol anhydrous ferric trichloride is added to 0.3mol 1- hexyl -3- first at a temperature of 20 DEG C under protection of argon gas
In base imidazoles villaumite, stirring 48h reacts it sufficiently, obtains molysite ionic liquid.
The triphenylamine (TPAn) of 0.6mol is added in above-mentioned molysite ionic liquid, under protection of argon gas 20 DEG C of stirrings
It reacts it sufficiently for 24 hours, filters, collect precipitating, wash precipitating three times with methanol, the precipitating after washing is placed in saturation ammonium hydroxide
In, poly-triphenylamine positive electrode is obtained by filtration after being stirred overnight.
As a positive electrode active material by obtained poly-triphenylamine positive electrode, it is sufficiently mixed with conductive agent acetylene black uniformly,
Poly-triphenylamine account for poly-triphenylamine, acetylene black, PVDF three's gross mass 60%, acetylene black accounts for the 20% of gross mass, stirs dry-mixed
Bonding agent PVDF is added after mixing uniformly, PVDF accounts for the 20% of gross mass, dry-mixed to add N-Methyl pyrrolidone after mixing evenly
Slurry is formed, the solid content for controlling slurry is 60%, and slurry viscosity 5500cps obtains anode sizing agent.Anode sizing agent is coated on
It on aluminium foil, is rolled on milling roller, poly-triphenylamine electrode is obtained after punching.
Embodiment 5
By 0.1mol 1- ethyl -3- methylimidazole villaumite, 0.1mol triethylamine hydrochloride, 0.1mol N- crassitude
Ketone villaumite and 0.1mol1- decyl -3- methylimidazole villaumite are uniformly mixed at 80 DEG C, obtain ionic liquid, under protection of argon gas
0.8mol anhydrous ferric trichloride is added in solution at a temperature of 80 DEG C, stirring 36h reacts it sufficiently, obtains molysite ion
Liquid.
The triphenylamine (TPAn) of 0.4mol is added in above-mentioned molysite ionic liquid, under nitrogen protection 80 DEG C of stirrings
It reacts it sufficiently for 24 hours, filters, collect precipitating, wash precipitating three times with methanol, the precipitating after washing is placed in saturation ammonium hydroxide
In, poly-triphenylamine positive electrode is obtained by filtration after being stirred overnight.
As a positive electrode active material by obtained poly-triphenylamine positive electrode, it is sufficiently mixed with conductive agent acetylene black uniformly,
Poly-triphenylamine account for poly-triphenylamine, acetylene black, PVDF three's gross mass 70%, acetylene black accounts for the 20% of gross mass, stirs dry-mixed
Bonding agent PVDF is added after mixing uniformly, PVDF accounts for the 10% of gross mass, dry-mixed to add N-Methyl pyrrolidone after mixing evenly
Slurry is formed, the solid content for controlling slurry is 50%, and slurry viscosity 5000cps obtains anode sizing agent.Anode sizing agent is coated on
It on aluminium foil, is rolled on milling roller, poly-triphenylamine electrode is obtained after punching.
Embodiment described above is only that preferred embodiment of the invention is described, and is not carried out to the scope of the present invention
It limits, without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention
Various changes and improvements, should all fall into claims of the present invention determine protection scope in.
Claims (10)
1. a kind of preparation method of polymer cathode materials for Li-ion battery, which comprises the following steps:
Triphenylamine is added in molysite ionic liquid, stirring 2~48h under inert gas protection reacts it sufficiently；Then, will
Solution is placed in methanol and stands 1~7 day, and filtering, gained precipitating is washed with methanol, after being stirred overnight in saturation ammonium hydroxide, filtering,
Up to poly-triphenylamine positive electrode.
2. a kind of preparation method of polymer cathode materials for Li-ion battery according to claim 1, which is characterized in that institute
The synthetic method for stating molysite ionic liquid is as follows: ionic liquid being uniformly mixed at a temperature of 20~100 DEG C, is protected in inert gas
Ferric trichloride is added in ionic liquid under shield, 2~48h of stirring reacts it sufficiently.
3. a kind of preparation method of polymer cathode materials for Li-ion battery according to claim 2, which is characterized in that institute
Stating ionic liquid is 1- allyl -3- methylimidazolium chloride villaumite, 1- decyl -3- methylimidazole villaumite, 1- octyl -3- methyl miaow
Azoles villaumite, 1- butyl -2,3- methylimidazole villaumite, 1- ethyl-3-methylimidazole villaumite, 1- hexyl -3- methylimidazole villaumite,
Or mixtures thereof one of N-Methyl pyrrolidone villaumite, triethylamine hydrochloride.
4. a kind of preparation method of polymer cathode materials for Li-ion battery according to claim 2, which is characterized in that institute
The molar ratio for stating ferric trichloride and ionic liquid is 1~2:1.
5. a kind of preparation method of polymer cathode materials for Li-ion battery according to claim 1, which is characterized in that institute
The molar ratio for stating the ferric trichloride and triphenylamine in molysite ionic liquid is 1~3:1.
6. gathering made from a kind of preparation method of the described in any item polymer cathode materials for Li-ion batteries of Claims 1 to 5
Triphenylamine positive electrode.
7. a kind of poly-triphenylamine positive electrode as claimed in claim 6 is preparing the application in poly-triphenylamine anode electrode, special
Sign is, includes the following steps,
(1) it the preparation of anode sizing agent: as a positive electrode active material by the poly-triphenylamine positive electrode, is filled with conductive agent acetylene black
It point is uniformly mixed, is stirring evenly and then adding into bonding agent PVDF dry-mixed, it is dry-mixed to add N- methylpyrrole after mixing evenly
Alkanone forms slurry, controls the solid content and slurry viscosity of slurry, obtains anode sizing agent；
(2) preparation of anode electrode: step (1) described anode sizing agent being coated on aluminium foil, is rolled on milling roller, punching
Poly-triphenylamine anode electrode is obtained after cutting.
8. poly-triphenylamine positive electrode according to claim 7 is preparing the application in poly-triphenylamine anode electrode, special
Sign is that the anode sizing agent includes following components in mass ratio, and poly-triphenylamine positive electrode accounts for 50%~80%, conductive agent second
Acetylene black accounts for 10%~30%, bonding agent PVDF and accounts for 10%~20%.
9. poly-triphenylamine positive electrode according to claim 7 is preparing the application in poly-triphenylamine anode electrode, special
Sign is that the solid content in the anode sizing agent is 40~60%, and slurry viscosity is 4500~6000cps.
10. the preparation method of polymer cathode materials for Li-ion battery described in a kind of any one of Claims 1 to 5 claim
Middle molysite ionic liquid recovery method, it is characterised in that:
Ionic liquid is quickly separated with most water using Magnetic Isolation means, then activation is added into molysite ionic liquid
4A type molecular sieve, the arrest reaction 24 hours molysite with a small amount of moisture in adion liquid, after being removed water after filtering
Ionic liquid, molecular sieve continue to use after can drying.
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| CN114784250A (en) * | 2022-05-07 | 2022-07-22 | 江苏大学 | Positive electrode material, electrode and chargeable and dischargeable aluminum ion battery |
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Application publication date: 20190510 |