CN105800582A - Method for preparing difluoro-lithium phosphate and lithium-ion battery non-aqueous electrolyte - Google Patents
Method for preparing difluoro-lithium phosphate and lithium-ion battery non-aqueous electrolyte Download PDFInfo
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- CN105800582A CN105800582A CN201610147533.1A CN201610147533A CN105800582A CN 105800582 A CN105800582 A CN 105800582A CN 201610147533 A CN201610147533 A CN 201610147533A CN 105800582 A CN105800582 A CN 105800582A
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
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- C01B25/445—Metaphosphates of alkali metals
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- H—ELECTRICITY
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- 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
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- 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
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- H01M10/0567—Liquid materials characterised by the additives
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Abstract
The invention discloses a method for preparing difluoro-lithium phosphate and a lithium-ion battery non-aqueous electrolyte.The method includes the steps that under protection of inert gas, an organic solvent serves as a reaction medium, lithium hexafluorophosphate and an ether compound are reacted in a reaction vessel with an inner layer containing a PFA protective layer or a PTFE protective layer, wherein the reacting temperature is 50 DEG C-150 DEG C, and the reacting time is 5 h-20 h; after reaction is finished, a product is filtered and dried to obtain the difluoro-lithium phosphate product.The invention further relates to the lithium-ion battery non-aqueous electrolyte of the difluoro-lithium phosphate prepared with the method.The lithium-ion battery non-aqueous electrolyte comprises 0.5%-2.0% of difluoro-lithium phosphate, 15%-20% of electrolyte salt and 80%-85% of organic solvent.The method for preparing the difluoro-lithium phosphate is easy to operate, mild in condition and convenient to purify, and the high-purity difluoro-lithium phosphate can be obtained.
Description
Technical field
The present invention relates to the preparation method of a kind of difluorophosphate and lithium ion battery non-aqueous electrolyte.
Background technology
In recent years, one of the basic research of lithium ion battery and application and development focus becoming new energy field, each flourishing state of the world all it can be used as the break-through point of next new industry to develop and study.Positive electrode, negative material, electrolyte and diaphragm material are the big critical materials of lithium ion battery four, and common electrolyte mainly has LiPF6、LiBF4、LiClO4、LiAsF6、LiCF3SO3、LiN(CF3SO2)2Deng, in carbonate based organic solvent, it is made into nonaqueous electrolyte by dissolving these electrolyte, wherein LiPF6It it is current most widely used a kind of electrolyte.
The lithium ion battery adopting nonaqueous electrolyte is dramatically different in battery behavior, because the reactivity of electrode surface changes with the composition of nonaqueous electrolytic solution.Specifically, the decomposition of electrolyte and side reaction can affect the durability (such as cyclicity and high-temperature storage characteristics etc.) of lithium ion battery, people have attempted to suppress electrolyte to decompose in active anode compartment or negative terminal surface by adding various additive in electrolyte, to prevent performance degradation.
Current research has shown that adding difluorophosphate in the electrolytic solution can improve the battery performances such as the low-temperature characteristics of lithium rechargeable battery, cycle characteristics, preservation characteristics.Such as, patent documentation 1 describes such technology, wherein adopts and comprises at least one selected from single lithium fluophosphate Li2PO3F and difluorophosphate LiPO2F2The nonaqueous electrolytic solution of additive.In the art, described additive and lithium react formation film on interface between a positive electrode and a negative electrode, thus suppressing electrolyte because contact with positive electrode active material and negative electrode active material and decompose.Therefore, self discharge is inhibited, and the storage characteristics after charging is improved.In patent documentation 2, disclose by via electrolyte adds and film effect that difluorophosphate is formed on electrolysis interface and improve high-temperature cycle.
Non-patent literature 1 adopts LiPF6Preparing difluorophosphate with water reaction, this reaction is not easily controlled, and can produce LiPO4F etc. affect the by-product of battery performance, and are not easily purified, and are difficult to obtain high purity product.Patent documentation 3 adopts P4O10Powder and LiF powdered reaction, due to solid-solid reaction, the mixing organic solvent of generation extracts, and this method yield is low, complicated operation, and easily forms by-product, is not suitable for industrialized production.Patent documentation 4 adopts lithium hexafluoro phosphate and silicon dioxide to react at 50 DEG C and produces and lithium fluophosphate, but until reaction terminates to need extremely for a long time, more specifically the time was more than three days.
The synthesis of above-mentioned difluorophosphate is excessively difficult, to such an extent as to not yet sets up the effective ways being suitable for industrial production；And by-product is more, it is difficult to prepare highly purified difluorophosphoric acid salt.
[1] patent documentation 1:JP-A-11-67270；
[2] patent documentation 2: No. 3439085 publications of Japan Patent；
[3] non-patent literature 3: " HydrolysisinthesystemLiPF6-propylenecarbonate-dimethylcarbonate-H2O》JournalofFluorineChemistry126(2005)27-31
[4] patent documentation 3: publication WO2012004187A1；
[5] patent documentation 4: Japan Patent 2005-219994 publication.
Summary of the invention
Present invention aim at the deficiency existing for prior art and the preparation method of a kind of difluorophosphate and the technical scheme of lithium ion battery non-aqueous electrolyte are provided, the method adopts raw material cheap and easy to get, preparation technology is simple, be prone to industrialized production, and the difluorophosphate purity of preparation is high.
In order to solve above-mentioned technical problem, the present invention adopts the following technical scheme that
A kind of preparation method of difluorophosphate, it is characterized in that including following step: under inert gas shielding, with organic solvent for reaction medium, make lithium hexafluoro phosphate and ether compound contain in the reaction vessel of PFA or PTFE protective layer at internal layer to react, the molal quantity of lithium hexafluoro phosphate and the volume ratio of solvent are more than 1.5mol/L, in ether compound, the molal quantity of ehter bond (C-O-C) and the ratio of the molal quantity of lithium hexafluoro phosphate are more than 2, reaction temperature is 50～150 DEG C, response time is 5～20h, by the product obtained by filtering, washing, dry and obtain difluorophosphate.
Preferably, noble gas is the one in nitrogen or argon.
Preferably, organic solvent is carbonate-based solvent or carboxylic acid esters solvent, and described carbonate-based solvent or described carboxylic acid esters solvent include dimethyl carbonate, diethyl carbonate, butyl acetate, ethyl acetate.
Preferably, ether compound is chain ether compound or cyclic ether compounds, chain ether compound such as ether, tertbutyl ether etc., and cyclic ether compounds is 18 crown-s 6, epoxy ether such as.
Preferably, reaction temperature is 80～150 DEG C.
Preferably, the response time is 10～15h.
Lithium ion battery non-aqueous electrolyte prepared by a kind of preparation method containing above-mentioned difluorophosphate, it is characterised in that include following component: difluorophosphate: 0.5～2.0%；Electrolytic salt: 15～20%；Organic solvent: 80～85%.Apply the battery cryogenic discharging characteristic of this electrolyte, the function admirable such as big electric current puts dot characteristics, High temperature storage characteristic and cycle characteristics.
Preferably, electrolytic salt is LiPF6、LiBF4、LiN(CF3SO2)3、LiBOB、LiC2F4(SO3)2、LiCF3CO2、LiCF3SO3、LiN(C2F5SO2)2、LiC(CF3SO2)3、LiCnF2n+1SO3(n≥2)、LiN(RfOSO2)2In one or more mixture, wherein RfFor C1～10Fluoroalkyl.
Preferably, organic solvent is one or more the mixture in diethyl carbonate, fluorinated ethylene carbonate, Allyl carbonate, methyl ethyl ester, methyl propionate, ethylene carbonate or dimethyl carbonate.
Due to the fact that and have employed technique scheme, have the advantages that
1, preparation process of the present invention is simple, reaction temperature and be beneficial to industrialization, product can be easily separated purification simultaneously, the difluorophosphate purity prepared is high, impurity content low (free acidity is lower than 71ppm), product purity is more than 99.5%, the difluorophosphate prepared meets additive prescription, can add directly as lithium-ion battery electrolytes additive；
2, three wastes recoverable of the present invention, by a series of process such as washing, distillation, rectification, reaction organic solvent can be recycled, and reduces production cost；
3, the lithium ion battery of the non-aqueous electrolyte for lithium ion cell containing the present invention has good chemical property, the capacity of lithium ion battery is at more than 12Ah, capacity restoration rate is more than 92%, and low temperature capacity conservation rate is more than 90%, and 2000 capability retentions are more than 90%.
Detailed description of the invention
nullThe preparation method of a kind of difluorophosphate of the present invention，Including following step: under inert gas shielding，Preferably，Noble gas is the one in nitrogen or argon，With organic solvent for reaction medium，Preferably，Organic solvent is carbonate-based solvent or carboxylic acid esters solvent,Described carbonate-based solvent or described carboxylic acid esters solvent include dimethyl carbonate、Diethyl carbonate、Butyl acetate、Ethyl acetate，Make lithium hexafluoro phosphate and ether compound contain in the reaction vessel of PFA or PTFE protective layer at internal layer to react，Preferably，Ether compound is chain ether compound or cyclic ether compounds，Chain ether compound such as ether、Tertbutyl ether etc.，Cyclic ether compounds is 18 crown-6 such as、Epoxy ether，The molal quantity of lithium hexafluoro phosphate and the volume ratio of solvent are more than 1.5mol/L,In ether compound, the molal quantity of ehter bond (C-O-C) and the ratio of the molal quantity of lithium hexafluoro phosphate are more than 2，Reaction temperature is 50～150 DEG C，Response time is 5～20h，Preferably，Reaction temperature is 80～150 DEG C，Response time is 10～15h，By the product obtained by filtering、Washing、Dry and obtain difluorophosphate.
Lithium ion battery non-aqueous electrolyte prepared by a kind of preparation method containing above-mentioned difluorophosphate, including following component: difluorophosphate: 0.5～2.0%；Electrolytic salt: 15～20%；Organic solvent: 80～85%.Apply the battery cryogenic discharging characteristic of this electrolyte, the function admirable such as big electric current puts dot characteristics, High temperature storage characteristic and cycle characteristics.
Preferably, electrolytic salt is LiPF6、LiBF4、LiN(CF3SO2)3、LiBOB、LiC2F4(SO3)2、LiCF3CO2、LiCF3SO3、LiN(C2F5SO2)2、LiC(CF3SO2)3、LiCnF2n+1SO3(n≥2)、LiN(RfOSO2)2In one or more mixture, wherein RfFor C1～10Fluoroalkyl.
Preferably, organic solvent is one or more the mixture in diethyl carbonate, fluorinated ethylene carbonate, Allyl carbonate, methyl ethyl ester, methyl propionate, ethylene carbonate or dimethyl carbonate.
Embodiment 1～5
Under nitrogen atmosphere is protected, in reactor, first add ether compound, be subsequently adding the organic solution containing finite concentration lithium hexafluoro phosphate, control reaction temperature, time and stir speed (S.S.).Reaction condition is in Table 1.
Above-mentioned reactant liquor is processed, adopts sucking filtration, washing, drying, obtain product.Reaction condition and analysis result are in Table 1.
Embodiment 6～10 and comparative example
The formula of the lithium ion battery non-aqueous electrolyte of difluorophosphate is in Table 2, and its preparation method is as follows:
In the glove box under argon shield, electrolytic salt is joined in organic solvent, mix homogeneously, add the difluorophosphate that in embodiment 1～5, any embodiment prepares, thus obtaining lithium ion battery non-aqueous electrolyte.
The formula of lithium ion battery non-aqueous electrolyte is in Table 2.
The preparation of positive pole
Prepare positive pole through the following steps: the acetylene black of the LiFePO4 of 90% weight, the polyvinylidene fluoride (PVdF) of 5% weight, and 5% weight mixed；Add N-Methyl pyrrolidone and form slurry；Slurry is coated on two surfaces of aluminum collector body, is then dried.
The preparation of negative pole
Prepare negative pole through the following steps: the CMC+SBR of the graphite powder of 90% weight and 10% weight is mixed to form slurry；This slurry is coated on a surface of copper collector body, is then dried.
The mixing of electrolyte
Prepare basic electrolyte through the following steps: in the glove box of dry argon gas, the vinylene carbonate of 2 weight portions is added in the mixed solvent of 100 weight portions, this mixed solvent is the mixed solvent (volumetric mixture ratio is 1: 3) of ethylene carbonate and Ethyl methyl carbonate, and comprises the LiPF that ratio is 1.25mol/L6.Adding 0,0.5%wt% in this basic electrolyte, 1wt%, the difluorophosphate that 2wt% is synthesized by embodiment 1, thus obtaining electrolyte.
The assembling of lithium secondary battery
It is respectively coated with above-mentioned electrolyte and impregnates above-mentioned positive pole, negative pole, and film thickness be 16 μm, voidage be 45%, average pore size be the biaxial orientation porous polyethylene membrane of 0.05 μm, then they are pressed the order stacking of negative pole, dividing plate, positive pole, dividing plate and negative pole.So obtained battery component is first placed between PET film；Then when extending to sandwich film direction, installing the binding post of positive pole and negative pole, described sandwich film is by obtaining by resin bed overlying aluminum layer；Then its vacuum being sealed, prepare the 10Ah soft-package battery of lamellar, lithium ion battery non-aqueous electrolyte performance test is as shown in table 3.
Capacity is evaluated
Battery is charged to 3.6V with 0.2C, is then discharged to 2.7V with 0.2C, to be initially formed.Thereafter, battery is charged to 3.6V with 0.5C, be then again discharged to 0.7V with 0.2C, to measure the discharge capacity under 0.2C.In this, the cut-off current (cutcurrent) during charging is set in 0.05C.
The discharge capacity (mAh/g) of the discharge capacity (mAh/g) that capacity restoration rate (%)=60 DEG C is stored after a week under 0.2C/under 0.2C.
The specific discharge capacity (mAh/g) of the specific discharge capacity (mAh/g) of-20 DEG C/lower 25 DEG C of 0.2C under low temperature capacity conservation rate (%)=0.2C
Discharge capacity (mAh/g) under the 1C of discharge capacity (mAh/g) under 1C after capability retention (%)=2000 time circulation/first.
Table 1 embodiment 1～5 reaction condition and result
Lithium ion battery non-aqueous electrolyte formula (by weight mark) of table 2 embodiment 6～10 and comparative example
The lithium ion battery non-aqueous electrolyte the performance test results that table 3 embodiment 6～10 and comparative example prepare
These are only specific embodiments of the invention, but the technical characteristic of the present invention is not limited thereto.Any based on the present invention, for realizing essentially identical technique effect, done ground simple change, equivalent replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (9)
1. the preparation method of a difluorophosphate, it is characterised in that include following step:
Under inert gas shielding; with organic solvent for reaction medium; make lithium hexafluoro phosphate and ether compound contain in the reaction vessel of PFA or PTFE protective layer at internal layer to react; the volume ratio of the molal quantity of described lithium hexafluoro phosphate and described solvent is more than 1.5mol/L; in described ether compound, the molal quantity of ehter bond (C-O-C) and the ratio of the molal quantity of described lithium hexafluoro phosphate are more than 2; reaction temperature is 50～150 DEG C; response time is 5～20h, and by filtering, wash, drying, the product obtained is obtained difluorophosphate.
2. the preparation method of a kind of difluorophosphate according to claim 1, it is characterised in that: described noble gas is the one in nitrogen or argon.
3. the preparation method of a kind of difluorophosphate according to claim 1, it is characterized in that: described organic solvent is carbonate-based solvent or carboxylic acid esters solvent, described carbonate-based solvent or described carboxylic acid esters solvent include dimethyl carbonate, diethyl carbonate, butyl acetate, ethyl acetate.
4. the preparation method of a kind of difluorophosphate according to claim 1, it is characterised in that: described ether compound is chain ether compound or cyclic ether compounds.
5. the preparation method of a kind of difluorophosphate according to claim 1, it is characterised in that: described reaction temperature is 80～150 DEG C.
6. the preparation method of a kind of difluorophosphate according to claim 1, it is characterised in that: the described response time is 10～15h.
7. the lithium ion battery non-aqueous electrolyte that prepared by the preparation method containing difluorophosphate as claimed in claim 1, it is characterised in that include following component: difluorophosphate: 0.5～2.0%；Electrolytic salt: 15～20%；Organic solvent: 80～85%.
8. the lithium ion battery non-aqueous electrolyte that prepared by the preparation method of a kind of difluorophosphate according to claim 7, it is characterised in that: described electrolytic salt is LiPF6、LiBF4、LiN(CF3SO2)3、LiBOB、LiC2F4(SO3)2、LiCF3CO2、LiCF3SO3、LiN(C2F5SO2)2、LiC(CF3SO2)3、LiCnF2n+1SO3(n≥2)、LiN(RfOSO2)2In one or more mixture, wherein RfFor C1～10Fluoroalkyl.
9. the lithium ion battery non-aqueous electrolyte that prepared by the preparation method of a kind of difluorophosphate according to claim 7, it is characterised in that: described organic solvent is one or more the mixture in diethyl carbonate, fluorinated ethylene carbonate, Allyl carbonate, methyl ethyl ester, methyl propionate, ethylene carbonate or dimethyl carbonate.
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| CN106744782A (en) * | 2017-01-04 | 2017-05-31 | 九江天赐高新材料有限公司 | The preparation method of difluorophosphoric acid salt |
| CN106785045A (en) * | 2017-03-22 | 2017-05-31 | 国网河南省电力公司电力科学研究院 | A kind of preparation method of difluorophosphate, lithium-ion battery electrolytes and ion battery |
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| CN108123172A (en) * | 2016-11-29 | 2018-06-05 | 宁德时代新能源科技股份有限公司 | Electrolyte and secondary lithium battery |
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| CN108997217A (en) * | 2017-06-06 | 2018-12-14 | 东莞东阳光科研发有限公司 | A kind of difluorophosphoric acid imidazole ion liquid and preparation method thereof, electrolyte and application |
| CN108997217B (en) * | 2017-06-06 | 2022-07-26 | 东莞东阳光科研发有限公司 | Difluorophosphoric acid imidazole ionic liquid, preparation method thereof, electrolyte and application |
| JP2019172475A (en) * | 2018-03-26 | 2019-10-10 | 三井化学株式会社 | Method for producing lithium difluorophosphate |
| JP7020749B2 (en) | 2018-03-26 | 2022-02-16 | 三井化学株式会社 | Method for producing lithium difluorophosphate |
| CN109449387A (en) * | 2018-09-28 | 2019-03-08 | 深圳市卓能新能源股份有限公司 | A kind of lithium ion battery and preparation method thereof |
| CN111137870A (en) * | 2018-11-06 | 2020-05-12 | 宁波氟创新能源科技有限公司 | Lithium difluorophosphate, preparation method thereof and lithium ion battery electrolyte |
| CN112678795A (en) * | 2019-10-18 | 2021-04-20 | 多氟多化工股份有限公司 | Preparation method of lithium difluorophosphate |
| CN114566712A (en) * | 2022-03-03 | 2022-05-31 | 湖北亿纬动力有限公司 | High-voltage lithium ion battery electrolyte containing lithium difluorophosphate, preparation method thereof and lithium ion battery |
| CN114566712B (en) * | 2022-03-03 | 2023-07-28 | 湖北亿纬动力有限公司 | High-voltage lithium ion battery electrolyte containing lithium difluorophosphate, preparation method thereof and lithium ion battery |
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