CN109286042B - Preparation method of electrolyte for lithium ion power battery - Google Patents
Preparation method of electrolyte for lithium ion power battery Download PDFInfo
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- CN109286042B CN109286042B CN201710598544.6A CN201710598544A CN109286042B CN 109286042 B CN109286042 B CN 109286042B CN 201710598544 A CN201710598544 A CN 201710598544A CN 109286042 B CN109286042 B CN 109286042B
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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
- H01M10/058—Construction or manufacture
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0568—Liquid materials characterised by the solutes
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a preparation method of electrolyte for a lithium ion power battery, and particularly relates to a preparation method of non-aqueous electrolyte for the lithium ion power battery. The method comprises the steps of firstly adding more than two non-aqueous solvents into an electrolyte preparation kettle, controlling the temperature and the pressure of materials, starting stirring, and adding electrolyte lithium salt LiPF according to the proportion requirement6Dissolving and mixing; then adding a small amount of other lithium salt (Li) into the electrolyte preparation kettle3PO4、Li2HPO4) Heating, stirring, dissolving, and vacuum treating; and finally, filtering the electrolyte into another preparation kettle, adding other functional additives in proportion, mixing and dissolving, and filtering to obtain a qualified product. The method is simple to operate and can inhibit LiPF6High-temperature decomposition and improvement of the high-temperature performance of the electrolyte; and the cost of the used raw materials is low, so that the method has high market application and popularization values.
Description
Technical Field
The invention relates to the technical field of electrolyte for a lithium ion power battery, in particular to a preparation method of the electrolyte for the lithium ion power battery.
Background
The application market of the lithium ion battery is divided into three parts, namely consumer electronics products, new energy power automobiles and energy storage. With the rapid development of electric automobiles and energy storage technologies in recent years, the market demand of the electrolyte serving as one of four key materials of lithium ion batteries is continuously increased. Meanwhile, the performance requirements of the battery are increasingly improved, and particularly, the power battery has higher requirements on capacity, cycle life and high-temperature characteristics.
The non-aqueous electrolyte for the power lithium ion battery is prepared by dissolving an electrolyte in two or more non-aqueous organic solvents, wherein the electrolyte plays a role of providing a conductive ion source. LiPF6The electrolyte for the lithium ion battery is the most widely used electrolyte for the lithium ion battery at present due to outstanding comprehensive performance. However, as the lithium ion battery continues to operate and heat up, LiPF6The following reactions occur:
the decomposition accelerates irreversible lithium consumption, the HF destroys the SEI film, and the HF reacts with the positive active material to form an insulating film, so that the capacity of the battery is quickly attenuated (the cycle life is short), and the battery deviates from the normal state, thereby causing safety problems.
Therefore, how to provide a LiPF suppressing agent6The preparation method of the electrolyte for the lithium ion power battery, which is decomposed at high temperature and improves the high-temperature performance of the electrolyte, is an urgent problem to be solved by technical personnel in the field.
Disclosure of Invention
In view of the above, the present invention provides a method for preparing an electrolyte for a lithium ion power battery, which belongs to a novel method for preparing a non-aqueous electrolyte for a lithium ion battery, and the method is characterized in that a lithium salt Li is introduced in the preparation process3PO4、Li2HPO4And LiPF6Heating and dissolving together to make LiPF6Premature decomposition to eliminate or inhibit LiPF6The electrolyte solution is heated and decomposed during use of the battery, thereby causing deterioration of the battery performance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of electrolyte for a lithium ion power battery comprises the following steps:
A. vacuum pretreatment of solvent raw materials: adding more than two kinds of non-aqueous organic solvents into an electrolyte preparation kettle according to the proportion requirement of the electrolyte formula, controlling the kettle temperature to be-20-60 ℃ and the pressure to be-0.02-0.1 MPa, starting stirring, wherein the stirring speed is 20-200 r/min, and the stirring time is 1-8 hours;
B. vacuum dissolution treatment of electrolyte salt: adding LiPF into the electrolyte preparation kettle in the step A according to the formula proportion requirement of the electrolyte6And 0.5 to 5%, preferably 1 to 2%, of Li is added3PO4Or Li2HPO4Heating and stirring the mixture in a vacuum environment to perform dissolution reaction; wherein the temperature of the kettle is controlled to be 0-60 ℃, the pressure is controlled to be-0.02-0.1 MPa, the stirring speed is 20-200 r/min, and the stirring time is 1-10 hours;
C. mixing and homogenizing functional additives: adding at least one functional additive with the concentration of 1-20% into the reaction system in the step B according to the formula proportion requirement of the electrolyte, and mixing and dissolving for 0.5-12 hours;
D. refining and filtering: and D, cooling the electrolyte treated in the step C to-5-20 ℃, preferably to 5-10 ℃, carrying out precision filtration, and packaging according to a specified amount to obtain a final product.
Preferably, in step a, the non-aqueous organic solvent includes an organic carbonate solvent and a non-carbonate solvent; wherein the organic carbonate-based solvent includes one or more of dimethyl carbonate (DMC), diethyl carbonate (DEC), Ethyl Methyl Carbonate (EMC), Ethylene Carbonate (EC), Propylene Carbonate (PC); the non-carbonate solvent includes one or more of Methyl Acetate (MA), Ethyl Acetate (EA), Propyl Acetate (PA), Methyl Propionate (MP), Ethyl Propionate (EP), Methyl Butyrate (MB), Ethyl Butyrate (EB).
Preferably, the nonaqueous organic solvent accounts for 10-90%, preferably 70-85% of the total mass of the electrolyte.
Preferably, in step C, the functional additive comprises a salt-type additive and an organic additive; wherein the solid salt additive comprises one or more of lithium tetrafluoroborate (LiBF4), lithium bis (oxalato) borate (LiBOB), lithium difluoro (oxalato) borate (LiODFB), lithium bis (fluorosulfonyl) imide (LiFSI), lithium bis (trifluoromethylsulfonyl) imide (LiTFSI), lithium carbonate (Li2CO3) and lithium perchlorate (LiClO 4); the organic additive comprises one or more of Vinylene Carbonate (VC), fluoroethylene carbonate (FEC), Vinyl Ethylene Carbonate (VEC), Fluoroether (FE), Propane Sultone (PS), Propene Sultone (PST), trifluoromethyl ethylene carbonate (TFPC), vinyl sulfate (DTD), Ethylene Sulfite (ES), Succinonitrile (SN), Adiponitrile (ADN), 4-methylbenzonitrile (4-TN), Biphenyl (BP), Cyclohexylbenzene (CHB), Fluorobenzene (FB) and 4-fluorotoluene (4-FT).
Preferably, the salt additive accounts for 1-20%, preferably 1-10% of the total mass of the electrolyte; the organic additive accounts for 0.5-15%, preferably 1-10% of the total mass of the electrolyte.
Preferably, in the step A, the temperature of the kettle is controlled to be-5-20 ℃, the pressure is controlled to be-0.07-0.09 MPa, the stirring speed is 60-150 r/min, and the stirring time is 2-4 hours, so as to remove fusel which is harmful to the battery performance in the solvent.
Preferably, in the step B, the temperature of the kettle is controlled to be 30-40 ℃, the pressure is-0.07-0.09 MPa, the stirring speed is 60-150 r/min, and the stirring time is 4-6 hours, so that part of lithium salt in the electrolyte is promoted to be decomposed in advance.
Preferably, in the step C, the dissolving time is 1-6 hours.
And comparing the treated electrolyte product with an untreated electrolyte product through detection and analysis. And detecting the contents of fusel, free acid, phosphorus oxytrifluoride, lithium fluoride and lithium phosphorus oxydifluoride in the solution before and after the treatment.
According to the technical scheme, compared with the prior art, the invention discloses the preparation method of the electrolyte for the lithium ion power battery, which is characterized in that in the preparation process of the electrolyte for the lithium ion battery, vacuum and heating processes are introduced, and a small amount of lithium salt Li is added3PO4、Li2HPO4Make LiPF6Heating to decompose in advance, reacting with trace water in electrolyte, and vacuum-pumping out trace HF generated during reaction to eliminate or inhibit LiPF6The electrolyte is decomposed by the temperature rise of the battery during use, and the battery performance is reduced.
The method not only has simple operation, but also can inhibit LiPF6High-temperature decomposition and improvement of the high-temperature performance of the electrolyte; and the cost of the used raw materials is low, so that the method has high market application and popularization values.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a flow chart of the method steps of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a preparation method of electrolyte for a lithium ion power battery, which is simple to operate and can inhibit LiPF6High-temperature decomposition and improvement of the high-temperature performance of the electrolyte; and the cost of the used raw materials is low, so that the method has high market application and popularization values.
The present invention will be further specifically illustrated by the following examples for better understanding, but the present invention is not to be construed as being limited thereto, and certain insubstantial modifications and adaptations of the invention by those skilled in the art based on the foregoing disclosure are intended to be included within the scope of the invention.
The content and indexes of each component of the reference electrolyte are as follows:
reference formula 1 electrolyte:
ethylene Carbonate (EC), Ethyl Methyl Carbonate (EMC), dimethyl carbonate (DMC) 1:1:1(W)
Lithium hexafluorophosphate (LiPF6) mass concentration: 12.5 percent of the total weight of the mixture,
VC mass concentration: 2.5 percent of the total weight of the mixture,
mass concentration of PS: 1.5 percent of the total weight of the mixture,
chroma (APHA) index: less than or equal to 50; (measurement value: 17)
Moisture (karl fischer method) index: less than or equal to 10 PPm; (measurement value: 5PPm)
Conductivity index: 10.45 +/-0.05 ms/cm; (measurement value: 10.47ms/cm)
Reference formula 2 electrolyte:
ethylene Carbonate (EC), Ethyl Methyl Carbonate (EMC), diethyl carbonate (DEC) ═ 1:1:1(V)
Lithium hexafluorophosphate (LiPF6) mass concentration: 13.5 percent
VC mass concentration: 2 percent of the total weight of the mixture,
mass concentration of PS: 2 percent of the total weight of the mixture,
chroma (APHA) index: less than or equal to 50; (measurement value: 16)
Moisture (karl fischer method) index: less than or equal to 10 PPm; (measurement value: 6PPm)
Conductivity index: 8.50 +/-0.05 ms/cm; (measurement value: 8.52ms/cm)
Comparative example 1
Preparing 1 ton of standard formula 1 electrolyte: sealing and pressing equal amount of low water raw materials including Ethyl Methyl Carbonate (EMC), Ethylene Carbonate (EC) and dimethyl carbonate (DMC) into 1m3Preparing a kettle, starting stirring, keeping the rotating speed at 100 rpm, opening a heat-conducting medium for controlling torsion, and setting the temperature of the kettle to be 5 ℃; after 1 hour, lithium hexafluorophosphate (LiPF6) and functional additives VC and PS are added in proportion, stirred and mixed for 4 hours, and then filtered, sampled and detected.
Example 1
Preparing 1 ton of standard formula 1 electrolyte: sealing and pressing equal amount of low water raw materials including Ethyl Methyl Carbonate (EMC), Ethylene Carbonate (EC) and dimethyl carbonate (DMC) into 1m3Preparing a kettle, starting stirring, keeping the rotating speed at 100 rpm, opening a heat-conducting medium to control torsion, setting the temperature of the preparing kettle to be 20 ℃, keeping the vacuum degree to be-0.8 MPa, and stirring and vacuumizing for 3 hours; then adding lithium hexafluorophosphate (LiPF) in proportion6) And 1.5% Li3PO4Setting the temperature of a preparation kettle at 50 ℃, keeping the vacuum degree at-0.8 MPa, stirring, vacuumizing for 6 hours, filtering, adding the functional additives VC and PS in proportion, stirring and mixing for 4 hours, filtering, sampling and detecting.
Comparative example 2
Preparing 1 ton of standard formula 2 electrolyte: sealing and pressing equal amount of low water raw materials such as Ethyl Methyl Carbonate (EMC), Ethylene Carbonate (EC) and diethyl carbonate (DEC) into the container for 1m3Preparing a kettle, starting stirring, keeping the rotating speed at 100 rpm, opening a heat-conducting medium for controlling torsion, and setting the temperature of the kettle to be 5 ℃; lithium hexafluorophosphate (LiPF) was added in proportion after 1 hour6) And functional additives VC and PS, stirring and mixing for 5 hours, filtering, sampling and detecting.
Example 2
Preparing 1 ton of standard formula 2 electrolyte: sealing and pressing equal amount of low water raw materials such as Ethyl Methyl Carbonate (EMC), Ethylene Carbonate (EC) and diethyl carbonate (DEC) into the container for 1m3Preparing a kettle, starting stirring, keeping the rotating speed at 100 rpm, opening a heat-conducting medium to control torsion, setting the temperature of the preparing kettle to be 20 ℃, keeping the vacuum degree to be-0.8 MPa, and stirring and vacuumizing for 3 hours; then adding lithium hexafluorophosphate (LiPF) in proportion6) And 1.5% Li3PO4Setting the temperature of a preparation kettle at 50 ℃, keeping the vacuum degree at-0.8 MPa, stirring, vacuumizing for 6 hours, filtering, adding the functional additives VC and PS in proportion, stirring and mixing for 4 hours, filtering, sampling and detecting.
Comparative test data are shown in the following table:
the result shows that the electrolyte prepared by the method has better technical indexes, and each index and performance completely meet the requirements of the lithium ion battery. Fusel and POF, in particular, which are detrimental to battery performance3The content is obviously reduced, and a new salt LiPO with obvious effect on the battery performance appears2F2。
Comparative and example cell performance test results
| Comparative example 1 | Example 1 | Comparative example 2 | Example 2 | |
| Retention of circulating capacity at 25 ℃ for 800 weeks% | 70.8 | 87.6 | 76.5 | 90.1 |
The result shows that the electrolyte prepared by the method of the invention has obvious improvement on the cycle performance of the battery after the electrolyte is injected and formed into the lithium ion battery.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. A preparation method of electrolyte for a lithium ion power battery is characterized by comprising the following steps:
A. vacuum pretreatment of solvent raw materials: adding more than two kinds of non-aqueous organic solvents into an electrolyte preparation kettle according to the proportion requirement of the electrolyte formula, controlling the kettle temperature to be-20-60 ℃ and the pressure to be-0.02 to-0.1 MPa, starting stirring, wherein the stirring speed is 20-200 r/min, and the stirring time is 1-8 hours;
B. vacuum dissolution treatment of electrolyte salt: adding LiPF into the electrolyte preparation kettle in the step A according to the formula proportion requirement of the electrolyte6And 0.5% -5% of Li is added3PO4Or Li2HPO4Heating and stirring the mixture in a vacuum environment to perform dissolution reaction; wherein the temperature of the kettle is controlled to be 30-50 ℃, the pressure is controlled to be-0.02 to-0.1 MPa, the stirring speed is 20-200 r/min, and the stirring time is 1-10 hours, so as to promote the decomposition of part of lithium salt in the electrolyte in advance;
C. mixing and homogenizing functional additives: adding at least one functional additive with the concentration of 1-20% into the reaction system in the step B according to the formula proportion requirement of the electrolyte, and mixing and dissolving for 0.5-12 hours;
D. refining and filtering: cooling the electrolyte treated in the step C to-5-20 ℃, performing precise filtration, and packaging according to a specified amount to obtain a final product;
in the step C, the functional additive comprises a salt additive and an organic additive; wherein the solid salt additive comprises lithium tetrafluoroborate (LiBF)4) Lithium bis (oxalato) borate (LiBOB), lithium difluoro (oxalato) borate (LiODFB), lithium bis (fluorosulfonyl) imide (LiFSI), lithium bis (trifluoromethylsulfonyl) imide (LiTFSI), lithium carbonate (Li)2CO3) Lithium perchlorate (LiClO)4) One or more of; the organic additive comprises one or more of Vinylene Carbonate (VC), fluoroethylene carbonate (FEC), Vinyl Ethylene Carbonate (VEC), Fluoroether (FE), Propane Sultone (PS), Propene Sultone (PST), trifluoromethyl ethylene carbonate (TFPC), vinyl sulfate (DTD), Ethylene Sulfite (ES), Succinonitrile (SN), Adiponitrile (ADN), 4-methylbenzonitrile (4-TN), Biphenyl (BP), Cyclohexylbenzene (CHB), Fluorobenzene (FB) and 4-fluorotoluene (4-FT);
and the salt additive accounts for 1-10% of the total mass of the electrolyte; the organic additive accounts for 0.5-15% of the total mass of the electrolyte.
2. The method for preparing the electrolyte for the lithium-ion power battery according to claim 1, wherein in the step A, the non-aqueous organic solvent comprises an organic carbonate solvent and a non-carbonate solvent; wherein the organic carbonate-based solvent includes one or more of dimethyl carbonate (DMC), diethyl carbonate (DEC), Ethyl Methyl Carbonate (EMC), Ethylene Carbonate (EC), Propylene Carbonate (PC); the non-carbonate solvent includes one or more of Methyl Acetate (MA), Ethyl Acetate (EA), Propyl Acetate (PA), Methyl Propionate (MP), Ethyl Propionate (EP), Methyl Butyrate (MB), Ethyl Butyrate (EB).
3. The preparation method of the electrolyte for the lithium ion power battery according to claim 2, wherein the nonaqueous organic solvent accounts for 10-90% of the total mass of the electrolyte.
4. The preparation method of the electrolyte for the lithium-ion power battery according to claim 1, wherein in the step A, the temperature of the reaction kettle is controlled to be-5 ℃ to 20 ℃, the pressure is controlled to be-0.07 to-0.09 MPa, the stirring speed is 60 to 150 revolutions per minute, and the stirring time is 2 to 4 hours, so as to remove fusel which is harmful to the battery performance in the solvent.
5. The method for preparing the electrolyte for the lithium-ion power battery according to claim 1, wherein in the step C, the dissolving time is 1-6 hours.
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Effective date of registration: 20220324 Address after: 300000 Shuanghe Road South, Beichen Economic Development Zone, Beichen District, Tianjin Patentee after: TIANJIN JINNIU POWER SOURCES MATERIAL Co.,Ltd. Patentee after: Tianjin Jinniu New Material Co., Ltd Address before: 300000 Shuanghe Road South, Beichen Economic Development Zone, Beichen District, Tianjin Patentee before: TIANJIN JINNIU POWER SOURCES MATERIAL Co.,Ltd. |