CN109841908A - A kind of high flame retardant preparation method of lithium ion battery - Google Patents
A kind of high flame retardant preparation method of lithium ion battery Download PDFInfo
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- CN109841908A CN109841908A CN201811566884.1A CN201811566884A CN109841908A CN 109841908 A CN109841908 A CN 109841908A CN 201811566884 A CN201811566884 A CN 201811566884A CN 109841908 A CN109841908 A CN 109841908A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of high flame retardant preparation method of lithium ion battery, and positive active material, fire retardant are uniformly mixed, and conductive agent, PVDF, NMP is added, and kneading stirs to get anode sizing agent, are coated on aluminium foil and obtain anode pole piece；Negative electrode active material, conductive agent, SBR, CMC, water are uniformly mixed, negative electrode slurry is obtained, is coated on copper foil and obtains cathode pole piece；It is toasted, enter the operations such as shell, injection electrolyte, aging, chemical conversion by anode pole piece, cathode pole piece, membrane winding poling group, lithium ion battery is made.Fire retardant is directly added in anode sizing agent, after thermal runaway occurs for battery, can inhibit or prevent combustion reaction by physically or chemically mode；Fire retardant only forms a film in anode, will not be lost in cathode, reduce the additive amount of fire retardant, mitigates the analysis lithium situation of battery cathode to a certain extent；Since the burning point of fire retardant is higher, original performance such as cycle performance, processing performance of battery will not be influenced by being added in anode sizing agent.
Description
Technical field
The present invention relates to preparation method of lithium ion battery, especially a kind of high flame retardant preparation method of lithium ion battery.
Background technique
Lithium ion battery because its specific capacity is high, self discharge is small, operating temperature range is wide, voltage platform is high, have extended cycle life,
Memory-less effect, it is environmentally friendly the features such as, be widely used to the fields such as electric vehicle, energy storage, digital electronic goods, but lithium
The security performance of battery is still to influence a major issue of its business application.
Currently, common lithium ion battery, electrolyte are liquid organic electrolyte mostly on the market, by electric conducting lithium salt, have
Solvent and some specific additive compositions.It is mostly alkylcarbonic acid esters compound there are commonly solvent, such as: carbonic acid two
Ethyl ester (DEC), propene carbonate (PC), ethylene carbonate (EC), glycol dinitrate ester (DME) and methyl ethyl carbonate (EMC) etc..
But the flash-point of these organic solvents is low, volatility is high, when lithium battery overcharges, micro-short circuit and needle thorn or squeeze when,
Lithium battery interior temperature quickly increases, and is very easy to that liquid organic electrolyte is made to burn, and even explodes to cause cells burst.
Flame-retardant additive can release the free radical with flame retardant property when heated, which can capture in gas phase
Hydroperoxyl radical or hydroxyl free radical make organic liquid electrolyte to prevent the chain reaction of hydroperoxyl radical or hydroxyl free radical
Burning can not carry out or be difficult to carry out, to improve the security performance of lithium ion battery.But fire retardant has been added directly into
Meeting in machine liquid electrolyte increases the polarization effect of lithium battery interior so that the increase of its viscosity, ionic conductivity variation, keeps lithium electric
The degradations such as the circulation in pond, aggravation cathode analyses lithium situation, thus limits application of the fire retardant in lithium battery.
Summary of the invention
Goal of the invention: in view of the above-mentioned problems, the object of the present invention is to provide a kind of high flame retardant lithium ion battery preparation sides
Method solves to add fire retardant and bring negative effect directly in liquid organic electrolyte, is not influencing lithium battery performance
Under the premise of, improve the security performance of lithium battery.
A kind of technical solution: high flame retardant preparation method of lithium ion battery, comprising the following steps:
Step 1: positive active material, fire retardant are uniformly mixed, and conductive agent, PVDF, NMP is added, and kneading is stirred
To anode sizing agent, anode sizing agent is coated on aluminium foil and obtains anode pole piece；
Step 2: negative electrode active material, conductive agent, SBR, CMC, water are uniformly mixed, negative electrode slurry is obtained, cathode is starched
Material, which is coated on copper foil, obtains cathode pole piece；
Step 3: toasted, enter shell, is injection electrolyte, old by anode pole piece, cathode pole piece, membrane winding poling group
The operations such as change, chemical conversion, are made lithium ion battery.
Further, the additional amount of the fire retardant is the 3~15% of the positive active material quality.
Further, the fire retardant is below one of or at least two mixtures: tributyl phosphate, phosphorus
Sour three (2- ethylhexyl) esters, tricresyl phosphate (2- chloroethyl) ester, tricresyl phosphate (bis- chloropropyl of 2,3-) ester, tricresyl phosphate (2,3- dibromo
Propyl) the alkyl acid phosphates esters such as ester, Pyrol99, tricresyl phosphate-diphenyl ester, tricresyl phosphate, triphenyl phosphate, phosphoric acid (2-
Ethylhexyl) aryl phosphates such as-diphenyl ester, the alkanes such as trimethylolpropane, the dicyclopentadienes class such as Niran acid anhydrides, bromination
The aliphatic halogenated hydrocarbons such as object, methylene bromide, trichlorobromomethane, two chlorobromomethanes, octabromodiphenyl base oxide, pentabromoethyl benzene,
The aromatic bromides such as tetrabromobisphenol A and other halides, tricresyl phosphate (dibromopropyl) ester and cyclohexane halide and its derivative,
Decabromodiphenyl oxide and its derivative, the inorganic fire retardantss such as tellurium compound, hydroxy Al, magnesium hydroxide, borate.
Further, the anode sizing agent is coated at a temperature of 90~130 DEG C, and PVDF and conductive agent is avoided to float,
Influence the peeling force and conductive agent dispersion effect of pole piece.
Further, the negative electrode slurry is coated at a temperature of 70~90 DEG C, avoids CMC and conductive agent from floating, shadow
Ring pole piece quality.
Further, the positive active material is LiMn2O4、LiCoO2、NCA、NCM811、NCM523、NCM111、
LiFePO4One of which or at least two mixture.
Further, the negative electrode active material be graphite, be artificial graphite, natural graphite, carbonaceous mesophase spherules its
It is middle a kind of or at least two mixture.
Further, the electrolyte is ethylene carbonate (C3H4O3), propene carbonate (C4H6O3), diethyl carbonate
(C5H10O3), dimethyl carbonate (C3H6O3), methyl ethyl carbonate (C4H8O3), lithium hexafluoro phosphate (LiPF6) one of which.
The utility model has the advantages that compared with prior art, the invention has the advantages that fire retardant is directly added in anode sizing agent,
After thermal runaway occurs for battery, it can be inhibited by physically or chemically mode or prevent combustion reaction, efficiently avoided
The uncontrolled burning of battery or explosion improve the safety performance of lithium battery；Fire retardant only forms a film in anode, will not be in cathode
Loss, reduces the additive amount of fire retardant, can also mitigate the analysis lithium situation of battery cathode to a certain extent, therefore will not shadow
The viscosity for ringing electrolyte, will not reduce the ionic conductivity of electrolyte, not will lead to the polarization of battery and the DC internal resistance of battery
Increase, not will lead to battery analysis lithium situation and aggravate；Since the burning point of fire retardant is higher, addition will not influence in anode sizing agent
Original performance such as cycle performance, the processing performance of battery, operating method is simple, is easily achieved.
Detailed description of the invention
Fig. 1 is the self-extinguishing time contrast curve chart of each embodiment and comparative example；
Fig. 2 is the normal-temperature circulating performance contrast curve chart of embodiment 1, comparative example 1a, comparative example 1b；
Fig. 3 is the normal-temperature circulating performance contrast curve chart of embodiment 2, comparative example 2a, comparative example 2b；
Fig. 4 is the normal-temperature circulating performance contrast curve chart of embodiment 3, comparative example 3a, comparative example 3b；
Fig. 5 is the normal-temperature circulating performance contrast curve chart of embodiment 4, comparative example 4a, comparative example 4b；
Fig. 6 is the normal-temperature circulating performance contrast curve chart of embodiment 5, comparative example 5a, comparative example 5b.
Specific embodiment
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Embodiment 1
A kind of high flame retardant preparation method of lithium ion battery, comprising the following steps:
Step 1: positive active material (NCM523), fire retardant (tributyl phosphate) are uniformly mixed, the addition of fire retardant
Amount is the 5% of positive active material quality, and conductive agent, PVDF, NMP is added, and kneading stirs to get anode sizing agent, 90~
Anode sizing agent is coated on aluminium foil at a temperature of 130 DEG C and obtains anode pole piece；
Step 2: negative electrode active material (artificial graphite), conductive agent, SBR, CMC, water are uniformly mixed, and obtain cathode slurry
Negative electrode slurry, is coated on copper foil at a temperature of 70~90 DEG C and obtains cathode pole piece by material；
Step 3: toasted, enter shell, is injection electrolyte, old by anode pole piece, cathode pole piece, membrane winding poling group
The operations such as change, chemical conversion, are made 4Ah soft-package battery.
For embodiment 1, design: comparative example 1a --- the difference from embodiment 1 is that, it is added without fire retardant；Comparative example
1b --- the difference from embodiment 1 is that, fire retardant is added without in anode sizing agent, it will be for the resistance of positive active material quality 5%
Combustion agent is added in electrolyte.
Embodiment 2
A kind of high flame retardant preparation method of lithium ion battery, comprising the following steps:
Step 1: by positive active material (NCM523 and NCM811 in mass ratio 1: 1 are mixed to get), fire retardant (phosphoric acid
Tributyl) it is uniformly mixed, the additional amount of fire retardant is the 7% of positive active material quality, and conductive agent, PVDF, NMP is added,
Kneading stirs to get anode sizing agent, and anode sizing agent is coated on aluminium foil at a temperature of 90~130 DEG C and obtains anode pole piece；
Step 2: negative electrode active material (artificial graphite), conductive agent, SBR, CMC, water are uniformly mixed, and obtain cathode slurry
Negative electrode slurry, is coated on copper foil at a temperature of 70~90 DEG C and obtains cathode pole piece by material；
Step 3: toasted, enter shell, is injection electrolyte, old by anode pole piece, cathode pole piece, membrane winding poling group
The operations such as change, chemical conversion, are made 4Ah lithium battery.
For embodiment 2, design: comparative example 2a --- the difference from example 2 is that, it is added without fire retardant；Comparative example
2b --- the difference from example 2 is that, fire retardant is added without in anode sizing agent, it will be for the resistance of positive active material quality 7%
Combustion agent is added in electrolyte.
Embodiment 3
A kind of high flame retardant preparation method of lithium ion battery, comprising the following steps:
Step 1: by positive active material (LiFePO4), fire retardant (tricresyl phosphate) be uniformly mixed, fire retardant
Additional amount is the 6.5% of positive active material quality, and conductive agent, PVDF, NMP is added, and kneading stirs to get anode sizing agent,
Anode sizing agent is coated on aluminium foil at a temperature of 90~130 DEG C and obtains anode pole piece；
Step 2: negative electrode active material (natural graphite), conductive agent, SBR, CMC, water are uniformly mixed, and obtain cathode slurry
Negative electrode slurry, is coated on copper foil at a temperature of 70~90 DEG C and obtains cathode pole piece by material；
Step 3: toasted, enter shell, is injection electrolyte, old by anode pole piece, cathode pole piece, membrane winding poling group
The operations such as change, chemical conversion, are made 3Ah lithium battery.
For embodiment 3, design: comparative example 3a --- the difference with embodiment 3 is, is added without fire retardant；Comparative example
3b --- the difference with embodiment 3 is, fire retardant is added without in anode sizing agent, will be for positive active material quality 6.5%
Fire retardant is added in electrolyte.
Embodiment 4
A kind of high flame retardant preparation method of lithium ion battery, comprising the following steps:
Step 1: positive active material (NCM811), fire retardant (trimethylolpropane) are uniformly mixed, and fire retardant adds
Entering 6% that amount is positive active material quality, and conductive agent, PVDF, NMP is added, kneading stirs to get anode sizing agent, 90~
Anode sizing agent is coated on aluminium foil at a temperature of 130 DEG C and obtains anode pole piece；
Step 2: negative electrode active material (artificial graphite), conductive agent, SBR, CMC, water are uniformly mixed, and obtain cathode slurry
Negative electrode slurry, is coated on copper foil at a temperature of 70~90 DEG C and obtains cathode pole piece by material；
Step 3: toasted, enter shell, is injection electrolyte, old by anode pole piece, cathode pole piece, membrane winding poling group
The operations such as change, chemical conversion, are made 4Ah lithium battery.
For embodiment 4, design: comparative example 4a --- the difference with embodiment 4 is, is added without fire retardant；Comparative example
4b --- the difference with embodiment 4 is, fire retardant is added without in anode sizing agent, will be for the resistance of positive active material quality 6%
Combustion agent is added in electrolyte.
Embodiment 5
A kind of high flame retardant preparation method of lithium ion battery, comprising the following steps:
Step 1: positive active material (NCM811), fire retardant (triphenyl phosphate) are uniformly mixed, the addition of fire retardant
Amount is the 14% of positive active material quality, and conductive agent, PVDF, NMP is added, and kneading stirs to get anode sizing agent, 90~
Anode sizing agent is coated on aluminium foil at a temperature of 130 DEG C and obtains anode pole piece；
Step 2: negative electrode active material (artificial graphite), conductive agent, SBR, CMC, water are uniformly mixed, and obtain cathode slurry
Negative electrode slurry, is coated on copper foil at a temperature of 70~90 DEG C and obtains cathode pole piece by material；
Step 3: toasted, enter shell, is injection electrolyte, old by anode pole piece, cathode pole piece, membrane winding poling group
The operations such as change, chemical conversion, are made 4Ah lithium battery.
For embodiment 5, design: comparative example 5a --- the difference with embodiment 5 is, is added without fire retardant；Comparative example
5b --- the difference with embodiment 5 is, fire retardant is added without in anode sizing agent, will be for the resistance of positive active material quality 14%
Combustion agent is added in electrolyte.
To the above various embodiments and comparative example, tested under the self-extinguishing time, cycle performance and different temperatures of battery respectively
Analyse lithium situation.
Fig. 1 show the self-extinguishing time contrast curve chart of each embodiment and comparative example, 1 curve of line style from left to right 3
Coordinate points respectively correspond embodiment 1, comparative example a1, comparative example b1, and 2~5 curve of line style is similarly.As it can be seen that being added without fire retardant
Comparative example, battery can be burned to always no combustible, and fire retardant, which is added, can be such that the burning time of battery is substantially reduced, and hinder
When firing agent addition in anode sizing agent, the anti-flammability of battery will not be made to be deteriorated.
Fig. 2 show the normal-temperature circulating performance contrast curve chart of embodiment 1, comparative example 1a, comparative example 1b, and Fig. 3 is shown
The normal-temperature circulating performance contrast curve chart of embodiment 2, comparative example 2a, comparative example 2b, Fig. 4 show embodiment 3, comparative example 3a,
The normal-temperature circulating performance contrast curve chart of comparative example 3b, Fig. 5 show the normal temperature circulation of embodiment 4, comparative example 4a, comparative example 4b
Performance comparison curve graph, Fig. 6 show the normal-temperature circulating performance contrast curve chart of embodiment 5, comparative example 5a, comparative example 5b, often
25 DEG C of Wen Zhiyue.As it can be seen that fire retardant addition will not make the cycle performance of battery be deteriorated substantially in anode sizing agent, but fire retardant
It is added in the electrolytic solution, due to reducing the ionic conductivity of electrolyte, the polarization effect of battery is increased, so that battery follows
There are many ring degradation.
Listed in Table is the analysis lithium situation of each embodiment and comparative example at different temperatures.As it can be seen that fire retardant is added just
In the slurry of pole, anode analysis lithium situation will not aggravate substantially, but fire retardant is added in the electrolytic solution, can make the kinetics of battery
It can be deteriorated, to aggravate anode analysis lithium.
Claims (8)
1. a kind of high flame retardant preparation method of lithium ion battery, it is characterised in that the following steps are included:
Step 1: positive active material, fire retardant are uniformly mixed, and conductive agent, PVDF, NMP is added, and kneading stirs to get just
Pole slurry, anode sizing agent is coated on aluminium foil and obtains anode pole piece；
Step 2: negative electrode active material, conductive agent, SBR, CMC, water are uniformly mixed, negative electrode slurry is obtained, negative electrode slurry is applied
Cloth obtains cathode pole piece on copper foil；
Step 3: toasted, enter shell, injection electrolyte, aging, change by anode pole piece, cathode pole piece, membrane winding poling group
It is operated at equal, lithium ion battery is made.
2. a kind of high flame retardant preparation method of lithium ion battery according to claim 1, it is characterised in that: the fire retardant
Additional amount be the positive active material quality 3~15%.
3. a kind of high flame retardant preparation method of lithium ion battery according to claim 1, it is characterised in that: the fire retardant
For below one of or at least two mixtures: tributyl phosphate, tri-2-ethylhexyl phosphate, tricresyl phosphate
The alkyl acid phosphates such as (2- chloroethyl) ester, tricresyl phosphate (bis- chloropropyl of 2,3-) ester, tricresyl phosphate (2,3- dibromopropyl) ester, Pyrol99
Esters, the aryl phosphoric acids such as tricresyl phosphate-diphenyl ester, tricresyl phosphate, triphenyl phosphate, phosphoric acid (2- ethylhexyl)-diphenyl ester
Base ester, the alkanes such as trimethylolpropane, the dicyclopentadienes class such as Niran acid anhydrides, the aliphatic halogenated hydrocarbons such as bromide, dibromo first
The aromatic bromides such as alkane, trichlorobromomethane, two chlorobromomethanes, octabromodiphenyl base oxide, pentabromoethyl benzene, tetrabromobisphenol A
And other halides, tricresyl phosphate (dibromopropyl) ester and cyclohexane halide and its derivative, decabromodiphenyl oxide and its derivative, tellurium
The inorganic fire retardantss such as compound, hydroxy Al, magnesium hydroxide, borate.
4. a kind of high flame retardant preparation method of lithium ion battery according to claim 1, it is characterised in that: the anode slurry
Material is coated at a temperature of 90~130 DEG C.
5. a kind of high flame retardant preparation method of lithium ion battery according to claim 1, it is characterised in that: the cathode slurry
Material is coated at a temperature of 70~90 DEG C.
6. a kind of high flame retardant preparation method of lithium ion battery according to claim 1, it is characterised in that: the anode is living
Property substance be LiMn2O4、LiCoO2、NCA、NCM811、NCM523、NCM111、LiFePO4One of which or at least two
Mixture.
7. a kind of high flame retardant preparation method of lithium ion battery according to claim 1, it is characterised in that: the cathode is living
Property substance be graphite, be artificial graphite, natural graphite, the one of which of carbonaceous mesophase spherules or at least two mixture.
8. a kind of high flame retardant preparation method of lithium ion battery according to claim 1, it is characterised in that: the electrolyte
For ethylene carbonate, propene carbonate, diethyl carbonate, dimethyl carbonate, methyl ethyl carbonate, lithium hexafluoro phosphate wherein one
Kind.
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| KR20230054310A (en) * | 2021-10-13 | 2023-04-24 | 선천 캡쳄 테크놀로지 컴퍼니 리미티드 | secondary battery |
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