CN107293785B - Non-combustible lithium ion battery electrolyte and preparation method thereof - Google Patents
Non-combustible lithium ion battery electrolyte and preparation method thereof Download PDFInfo
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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
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- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention provides a non-combustible lithium ion battery electrolyte and a preparation method thereof, wherein the electrolyte consists of four components: (A) lithium salt, (B) organic solvent of carbonate and/or ether, (C) flame retardant additive of trifluoropropylmethyl cyclotrisiloxane and (D) other functional additive. Wherein, the molar concentration range of the lithium salt in the electrolyte is as follows: 0.001-2 mol/L; the mass ratio range of the flame retardant additive in the electrolyte is as follows: 0.1% -60%; the molar concentration ranges of other functional additives in the electrolyte are: 0.01-0.5 mol/L; the flame retardant additive is trifluoropropylmethylcyclotrisiloxane. According to the invention, trifluoropropyl methyl cyclotrisiloxane is used as a flame retardant additive, and trifluoropropyl methyl cyclotrisiloxane has two flame retardant elements of F and Si, so that the flame retardant additive has a synergistic effect, the additive dosage can be reduced, and the flame retardant efficiency can be improved.
Description
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to an electrolyte of a non-combustible lithium ion battery and a preparation method thereof.
Background
The lithium ion battery has the advantages of high energy density, good cycle stability, low self-discharge and the like, so the lithium ion battery becomes a research hotspot in the field of new energy and is the most probably marketable new energy.
However, in practical applications, there are many problems to be solved, such as volume change during charging and discharging, conductive lithium dendrite of material, etc. which affect the cycle performance and safety of the battery.
Lithium ion batteries can be subject to safety problems such as ignition, combustion and even explosion under abuse conditions such as overcharge, short circuit, violent impact, heat exposure, etc. The electrolyte, which is one of the important components of the battery, is also an important factor causing a problem in the safety of the battery. Because the potential of the negative electrode of the lithium ion battery is close to lithium, is more active and is unstable in an aqueous solution system, a non-aqueous and non-protonic organic solvent is required to be used as a carrier of lithium ions, and the lithium ion battery mostly adopts carbonates, ethers, carboxylates and/or sulfur-containing organic solvents as the carrier at present, the carbonate and/or ether organic solvent has the defects of low boiling point, easy volatilization, easy flammability, easy explosion and the like of the battery, for example, patent CN101867065 discloses a flame-retardant electrolyte solution containing organic solvents of carbonates and/or ethers, which provides a flame-retardant electrolyte solution with flame-retardant and even completely non-combustible functions, but it was found that after adding the flame-retardant additive, although the flame retardant performance is improved, the flame retardant performance has an influence on the battery capacity of the lithium battery, and the requirement on the high battery performance of the lithium battery cannot be met.
Therefore, in order to overcome the defects of the flame-retardant electrolyte containing carbonate and/or ether organic solvents in the prior art, it is necessary to further develop a new flame-retardant additive and a flame-retardant lithium ion battery electrolyte.
Disclosure of Invention
In order to overcome the defects, the invention provides the non-combustible lithium ion battery electrolyte and the preparation method thereof, which can improve the safety of the lithium ion battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides application of trifluoropropyl methyl cyclotrisiloxane in preparation of a non-combustible lithium ion battery or electrolyte thereof.
The invention also provides a non-combustible lithium ion battery electrolyte, which comprises: a flame retardant additive;
the flame retardant additive is trifluoropropylmethylcyclotrisiloxane.
Preferably, the trifluoropropylmethylcyclotrisiloxane has a mass fraction of 0.1% -60% in the electrolyte.
Preferably, the electrolyte further comprises: lithium salt, organic solvent of carbonate and/or ether and other functional additives.
Preferably, the molar ratio of the lithium salt to other functional additives is 0.001-2: 0.01 to 0.5.
Preferably, the lithium salt is LiPF6、LiClO4、LiAsF6、LiBF4、LiCH3SO3、LiCF3SO3LiBOB and LiN (CF)3SO2)2A mixture of one or more of them.
Preferably, the carbonate organic solvent is a cyclic carbonate and/or a chain carbonate compound;
preferably, the ether organic solvent is one or more selected from tetrahydrofuran, 2-methyltetrahydrofuran, 1, 3-dioxolane, dimethoxymethane, 1, 2-dimethoxyethane and diglyme
Preferably, the other functional additives are one or more of the following compounds: biphenyl, vinylene carbonate, vinyl ethylene carbonate, fluoroethylene carbonate, propylene sulfite, butylene sulfite, 1,3- (1-propene) sultone, ethylene sulfite, vinyl sulfate, cyclohexylbenzene, tert-butylbenzene, tert-amylbenzene and succinonitrile.
Preferably, the cyclic carbonate compound is one or more of ethylene carbonate, propylene carbonate, gamma-butyrolactone and butylene carbonate;
preferably, the chain carbonate compound is one or more selected from dimethyl carbonate, diethyl carbonate, dipropyl carbonate, methyl ethyl carbonate, and carbonate derivatives synthesized from linear or branched aliphatic monoalcohols having 3 to 8 carbon atoms and carbonic acid.
The invention also provides a preparation method of the non-combustible lithium ion battery electrolyte, which comprises the following steps:
dissolving lithium salt in organic solvent of carbonate and/or ether, adding trifluoro propyl methyl cyclotrisiloxane, and mixing thoroughly.
The invention also provides application of the trifluoropropyl methylcyclotrisiloxane or any one of the above non-combustible lithium ion battery electrolytes in preparing a button cell.
The invention has the advantages of
(1) The invention effectively reduces the release of inflammable gas, obviously improves the flash point of the lithium ion battery electrolyte and effectively solves the inflammable problem of the electrolyte.
(2) The electrolyte has high chemical stability and good reversible performance of battery charge and discharge.
(3) The preparation method is simple, strong in practicability and easy to popularize.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
A non-combustible lithium ion battery electrolyte is composed of four types of components: 0.001-2mol/L of lithium salt, carbonate and/or ether organic solvent, 0.1-60% of trifluoropropylmethyl cyclotrisiloxane flame retardant additive and 0.01-0.5mol/L of other functional additives.
Preferably, the trifluoropropylmethylcyclotrisiloxane flame retardant additive has the following structural formula:
preferably, the lithium salt is LiPF6、LiClO4、LiAsF6、LiBF4、LiCH3SO3、LiCF3SO3LiBOB (lithium bis (oxalato) borate) and LiN (CF)3SO2)2Or a mixture thereof.
Preferably, the carbonate organic solvent is a cyclic carbonate and/or a chain carbonate compound.
Further preferably, the cyclic carbonate compound is one or more of Ethylene Carbonate (EC), Propylene Carbonate (PC), gamma-butyrolactone (GBL) and butylene carbonate.
The chain carbonate compound is preferably selected from one or more of dimethyl carbonate (DMC), diethyl carbonate (DEC), dipropyl carbonate, methyl ethyl carbonate (EMC) and carbonate derivatives synthesized by straight chain or branched chain aliphatic monoalcohol with 3-8 carbon atoms and carbonic acid.
The ether organic solvent is one or more selected from Tetrahydrofuran (THF), 2-methyltetrahydrofuran, 1, 3-dioxolane, dimethoxymethane, 1, 2-dimethoxyethane and diglyme.
Other functional additives are one or more of the following compounds: biphenyl (BP), Vinylene Carbonate (VC), Vinyl Ethylene Carbonate (VEC), fluoroethylene carbonate (FEC), propylene sulfite, butylene sulfite, 1,3- (1-propene) sultone, Ethylene Sulfite (ES), vinyl sulfate, cyclohexylbenzene, tert-butylbenzene, tert-pentylbenzene, and succinonitrile.
The invention also provides a preparation method of the non-combustible lithium ion battery electrolyte, which comprises the following steps:
the flame retardant additive is dissolved in an organic solvent after being dewatered, and then lithium salt is added into the solvent containing the flame retardant additive and other functional additives in an anhydrous and oxygen-free environment to prepare electrolytes with different concentrations. The lithium salt should be added slowly to the solvent containing the flame retardant additive and other functional additives to prevent the solvent from boiling due to overheating.
The invention also protects the button cell prepared by using the non-combustible lithium ion battery electrolyte.
As introduced in the background art, the lithium ion battery electrolyte in the prior art has the disadvantages that the flame retardant effect and the battery performance cannot be improved simultaneously, and in order to solve the technical problems, the invention provides the non-combustible lithium ion battery electrolyte, wherein the electrolyte contains a phosphazene derivative flame retardant additive, the flame retardant additive is trifluoropropylmethylcyclotrisiloxane, and the structural formula of the flame retardant additive is as follows:
the electrolyte disclosed by the invention has the greatest characteristic of containing the trifluoropropyl methyl cyclotrisiloxane which is a flame-retardant additive, and the trifluoropropyl methyl cyclotrisiloxane has lower viscosity and can ensure high conductivity of the electrolyte; the flame-retardant alloy has two flame-retardant elements of F and Si, and the elements have a synergistic effect, so that the dosage of the additive can be reduced, as in example 18 and example 24, when the content of the flame-retardant alloy reaches 6% or 7%, the flame-retardant alloy has a completely non-flammable effect, and the flame-retardant efficiency is improved; the existence of the F element is beneficial to forming an excellent SEI film on an electrode interface, the compatibility between the electrolyte and an active material is improved, and the F element can also weaken the viscosity force between molecules, so that the migration resistance of the molecules and ions is reduced, the viscosity is further reduced, and the conductivity of the electrolyte is improved. The Si element has temperature resistance and high thermal stability, so that the electrolyte can resist high temperature and low temperature and can be used in a wide temperature range. The change with temperature is small whether the chemical property or the physical and mechanical property is changed. Has weather resistance and is not easily decomposed by ultraviolet light and ozone. The Si element has better thermal stability and radiation and weather resistance than other materials. The adopted trifluoropropylmethyl cyclotrisiloxane annular structure effectively connects the two flame-retardant elements together, so that not only is the battery performance of the lithium battery not negatively affected, but also the cycling stability and the battery capacity retention rate of the battery can be improved. Tests show that the two flame-retardant elements are connected together by adopting a trifluoropropylmethylcyclotrisiloxane annular structure, the flame-retardant elements are compact, the using amount of the flame-retardant additive is reduced, the flame-retardant effect is excellent, and the cycling stability and the capacity retention rate of the battery are improved.
Specifically, the electrolyte of the non-combustible lithium ion battery consists of four components: lithium salt, organic solvents of carbonates and/or ethers, a trifluoropropylmethyl cyclotrisiloxane flame-retardant additive and other functional additives;
wherein the molar concentration range of the lithium salt in the electrolyte is as follows: 0.001-2 mol/L.
The trifluoropropylmethyl cyclotrisiloxane flame-retardant additive accounts for the following mass fraction ranges in the electrolyte: 0.1% -60%;
the molar concentration ranges of other functional additives in the electrolyte are: 0.01-0.5 mol/L.
Preferably, the lithium salt is LiPF6、LiClO4、LiAsF6、LiBF4、LiCH3SO3、LiCF3SO3LiBOB (lithium bis (oxalato) borate) and LiN (CF)3SO2)2Or a mixture thereof.
Preferably, the carbonate organic solvent is a cyclic carbonate and/or a chain carbonate compound.
Further preferably, the cyclic carbonate compound is one or more of ethylene carbonate, propylene carbonate, gamma-butyrolactone and butylene carbonate.
The chain carbonate compound is preferably one or more of dimethyl carbonate, diethyl carbonate, dipropyl carbonate, methyl ethyl carbonate and carbonate derivatives synthesized by straight chain or branched chain aliphatic monoalcohol with 3-8 carbon atoms and carbonic acid.
The ether organic solvent is one or more selected from tetrahydrofuran, 2-methyltetrahydrofuran, 1, 3-dioxolane, dimethoxymethane, 1, 2-dimethoxyethane and diglyme.
Other functional additives are one or more of the following compounds: biphenyl (BP), Vinylene Carbonate (VC), Vinyl Ethylene Carbonate (VEC), fluoroethylene carbonate (FEC), propylene sulfite, butylene sulfite, 1,3- (1-propene) sultone, Ethylene Sulfite (ES), vinyl sulfate, cyclohexylbenzene, tert-butylbenzene, tert-pentylbenzene, and succinonitrile.
The invention also provides a preparation method of the non-combustible lithium ion battery electrolyte, which comprises the following steps:
the flame retardant additive is dissolved in an organic solvent after being dewatered, and then lithium salt is added into the solvent containing the flame retardant additive and other functional additives in an anhydrous and oxygen-free environment to prepare electrolytes with different concentrations. The lithium salt should be added slowly to the solvent containing the flame retardant additive and other functional additives to prevent the solvent from boiling due to overheating.
The invention also protects the button cell prepared by using the non-combustible lithium ion battery electrolyte.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
The invention lists the composition of 32 flame-retardant electrolyte solutions and the self-extinguishing time test data of each electrolyte solution in a table form, as shown in the following table 1.
TABLE 1 composition of various electrolytes, self-extinguishing time
As can be seen from table 1, the addition of the trifluoropropylmethylcyclotrisiloxane flame retardant additive to the electrolyte of the present invention can significantly improve the flame retardant performance of the electrolyte, such as the electrolyte in example 18, in which the volume ratio of the organic solvent is 1: 1: 1 EC/DEC/EMC with 0.3mol/L LiClO40.2mol/L VC and 6% of trifluoropropylmethylcyclotrisiloxane flame retardant additive can achieve the complete non-flammable effect (the self-extinguishing time is 0s), the flame retardant additive in the prior art can have a better non-flammable effect only when the mass fraction of the flame retardant additive in the electrolyte generally reaches 10-40%, but the flame retardant additive with higher mass fraction can increase the viscosity of the electrolyte, influence the conductivity of the electrolyte and further influence the battery performance of the lithium battery.
It can be seen from table 1 that different organic solvents and other functional additives have different effects on the flame retardant performance of the electrolyte, and the optimal electrolyte formulations obtained by screening and optimization are example 18 and example 14, and when the content of the flame retardant additive is low, the electrolyte can achieve a completely non-flammable effect.
Example 33
The electrolyte described in example 18 was injected into commercial LiMn2O4The charge and discharge experiment is carried out in the graphite lithium ion battery. It was found that after 20 weeks of battery cycle, the capacity retention of the battery without the flame retardant additive was 90%, and the capacity retention of the battery with the flame retardant additive was 94%.
The electrolyte described in example 24 was injected into commercial LiMn2O4The charge and discharge experiment is carried out in the graphite lithium ion battery. It was found that the capacity retention of the battery to which no flame retardant additive was added was 89%, and the capacity retention of the battery containing the flame retardant additive was 93% after the battery was cycled for 20 weeks.
The flame retardant additives in the prior art can reduce the flammability of the electrolyte, but most of the flame retardant additives have large negative effects on the battery performance of the lithium battery, and a few flame retardant additives can also reduce the battery performance of the lithium battery. After the flame retardant additive is added, a small amount of flame retardant additive is added on the premise of ensuring excellent flame retardant effect, so that not only is the battery performance of the lithium battery not negatively affected, but also the cycle stability and the battery capacity retention rate of the battery can be improved, and the flame retardant additive can be used as a safety additive to be applied to an actual battery, which is a technical effect that the conventional flame retardant additive for lithium battery electrolyte in the prior art cannot achieve and a technical effect that cannot be expected by a person skilled in the art. When the content of the flame retardant additive is high, the conductivity of the electrolyte, the cycle stability of the battery and the capacity retention rate of the battery are affected.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (1)
1. An application of trifluoropropyl methyl cyclotrisiloxane as flame-retarding additive in preparing the electrolyte of non-combustible Li-ion battery,
the mass fraction of the flame retardant additive trifluoropropylmethylcyclotrisiloxane is 6% or 7%;
the electrolyte further includes: lithium salt, organic solvents of carbonates and/or ethers and other functional additives;
the molar ratio of the lithium salt to other functional additives is 0.001-2: 0.01 to 0.5;
the lithium salt is LiPF6、LiClO4、LiAsF6、LiBF4、LiCF3SO3LiBOB and LiN (CF)3SO2)2A mixture of one or more of;
the carbonate organic solvent is a cyclic carbonate and/or a chain carbonate compound;
the ether organic solvent is one or more selected from tetrahydrofuran, 2-methyltetrahydrofuran, 1, 3-dioxolane, dimethoxymethane, 1, 2-dimethoxyethane and diglyme;
the other functional additives are one or more of the following compounds: biphenyl, vinylene carbonate, ethylene carbonate, fluoroethylene carbonate, propylene sulfite, butylene sulfite, 1-propylene-1, 3-sultone, ethylene sulfite, vinyl sulfate, cyclohexylbenzene, tert-butylbenzene, tert-amylbenzene;
the cyclic carbonate compound is one or more of ethylene carbonate, propylene carbonate and gamma-butyrolactone;
the chain carbonate compound is selected from one or more of dimethyl carbonate, diethyl carbonate, dipropyl carbonate and carbonate derivatives synthesized by straight chain or branched chain aliphatic mono-alcohol with the carbon number of 3-8 and carbonic acid.
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| CN109053792B (en) * | 2018-07-18 | 2021-03-12 | 石家庄圣泰化工有限公司 | Cyclic silicate compound for battery electrolyte and preparation method thereof |
| CN109004279A (en) * | 2018-07-18 | 2018-12-14 | 石家庄圣泰化工有限公司 | Application of the cyclic silicate ester compounds in battery electrolyte |
| CN110808411B (en) * | 2018-08-06 | 2022-07-12 | 宁德时代新能源科技股份有限公司 | Electrolyte and lithium ion battery |
| CN110931863B (en) * | 2019-11-12 | 2022-03-29 | 深圳市比克动力电池有限公司 | Additive for battery electrolyte, lithium ion battery electrolyte and lithium ion battery |
| CN111883831A (en) * | 2020-07-24 | 2020-11-03 | 香河昆仑化学制品有限公司 | Lithium ion battery electrolyte, battery cathode and electrochemical energy storage device |
| CN113346140A (en) * | 2021-06-01 | 2021-09-03 | 昆山宝创新能源科技有限公司 | Electrolyte and application thereof |
| CN113471537B (en) * | 2021-06-23 | 2022-11-01 | 绍兴铋华科技有限公司 | Flame-retardant electrolyte for lithium iron phosphate battery |
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