CN114221030B - Lithium ion battery electrolyte - Google Patents

Lithium ion battery electrolyte Download PDF

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Publication number
CN114221030B
CN114221030B CN202111305179.8A CN202111305179A CN114221030B CN 114221030 B CN114221030 B CN 114221030B CN 202111305179 A CN202111305179 A CN 202111305179A CN 114221030 B CN114221030 B CN 114221030B
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pvp
lithium
electrolyte
heteropolyblue
polyacid
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CN114221030A (en
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廖小东
***
黄兴兰
阮晓莉
李明科
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Dongfang Electric Group Research Institute of Science and Technology Co Ltd
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Dongfang Electric Group Research Institute of Science and Technology Co Ltd
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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
    • 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
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M10/0569—Liquid materials characterised by the solvents
    • 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
    • H01M2300/0028—Organic electrolyte characterised by the solvent
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Secondary Cells (AREA)

Abstract

The invention discloses a lithium ion battery electrolyte, which relates to the technical field of lithium ion batteries and is prepared by adding heteropolyblue lithium salt and a water locking agent into an organic solvent and dissolving the heteropolyblue lithium salt and the water locking agent in the organic solvent, so that the quantity of lithium ions in the battery is increased, and the service life of the battery is prolonged.

Description

Lithium ion battery electrolyte
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to lithium ion battery electrolyte.
Background
Lithium ion batteries are common secondary batteries in the market, and the main application range is in power batteries, energy storage batteries and 3C products. Lithium ion batteries operate primarily by virtue of lithium ions moving between a positive electrode and a negative electrode. During charge and discharge, li + Between two electrodes, li is inserted and removed back and forth during charging + De-intercalation from the positive electrode, and intercalation into the negative electrode through the electrolyte, wherein the negative electrode is in a lithium-rich state; the opposite is true when discharging.
The lithium ion battery electrolyte is one of the main materials of the lithium ion battery, determines the electrical performance of lithium ions like other main materials of the lithium ion battery, and is an indispensable important part in the link of lithium ion battery materials. The lithium battery electrolyte is a carrier for ion transmission in the battery and generally consists of lithium salt and an organic solvent, plays a role in conducting ions between the anode and the cathode of the lithium battery, ensures that the lithium battery has the advantages of high voltage, high specific energy and the like, and is generally prepared from high-purity organic solvent, electrolyte lithium salt, necessary additives and the like according to a certain proportion under certain conditions.
The electrolyte salt used in the lithium ion battery electrolyte is mainly lithium hexafluorophosphate, lithium tetrafluoroborate and the like, anions of the electrolyte salt are all negative monovalent, lithium ions matched with anions of 1 unit are 1 unit, and conventionally, the anions cannot carry more lithium ions. The attenuation mechanism of the lithium ion battery in the gradual use process is limited in the aspect of electrolyte, so that the lithium ion battery has a limited amount of lithium ions, and if the salt with 1 unit of anions capable of carrying a plurality of units of lithium ions is doped as electrolyte salt, the amount of lithium ions in the battery can be increased, and the service life of the battery is prolonged.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the lithium ion battery electrolyte which is prepared by adding heteropolyblue lithium salt and a water-locking agent and dissolving the heteropolyblue lithium salt and the water-locking agent in an organic solvent, so that the quantity of lithium ions in the battery is increased, and the service life of the battery is prolonged.
The invention provides lithium ion battery electrolyte, which comprises the following components:
the organic solvent accounts for 85-95% of the mass of the mixture, and the organic solvent is one or more of dimethyl carbonate, diethyl carbonate, ethylmethyl carbonate, propylene carbonate and ethylene carbonate;
the heteropolyblue electrolyte salt with the mass ratio of 10% -20% is Li 3 XY 12 O 40 Or Li (lithium) 4 XY 12 O 40 A lithium polyacid salt of a reduced structure, wherein X is a silicon element Si or a phosphorus element P, and Y is a tungsten element W or a molybdenum element Mo;
the water-locking agent accounts for 0% -2% of the mass of the water-locking agent, and the water-locking agent is polyvinylpyrrolidone (PVP) which comprises one or more of PVP-K12, PVP-K15, PVP-K17, PVP-K25, PVP-K30, PVP-K45, PVP-K60, PVP-K70, PVP-K80, PVP-K85, PVP-K90, PVP-K100, PVP-K110, PVP-K120 and PVP-K150.
Further, the heteropolyblue electrolyte salt is prepared by mixing polyacid H 3 XY 12 O 40 1 mol/liter aqueous solution, and 0.5 mol/liter lithium sulfiteIs an aqueous solution of (a); and then the prepared lithium sulfite solution is dripped into the polyacid solution, so that the strong oxidizing property of the polyacid solution oxidizes sulfite, the polyacid is reduced into heteropolyblue, and meanwhile, lithium ions in the lithium sulfite are attracted by negative charges of the heteropolyblue to form the heteropolyblue lithium salt.
Preferably, the lithium sulfite solution obtained by configuration is dripped into the polyacid solution to react for 4 hours to obtain the heteropolyblue electrolyte salt, and the obtained heteropolyblue electrolyte salt is dried at the temperature of 40 ℃ for standby.
More preferably, the organic solvent, the heteropolyblue electrolyte salt and the water-locking agent are prepared in advance respectively, and then the heteropolyblue electrolyte salt and the water-locking agent are added into the organic solvent according to the respective mass ratio to form the lithium ion battery electrolyte.
Compared with the prior art, the heteropoly blue lithium salt is a reduced state of the polyacid lithium salt, the polyacid lithium salt is reported to be used as electrolyte salt of a lithium ion battery in recent years, and after the polyacid lithium salt is reduced, anions obtain electrons, so that the negative charge quantity of the anions is increased, and the quantity of lithium ions carried by the anions is more.
The lithium ion electrolyte cannot contain water, the water content in the lithium battery is strictly controlled in the preparation process, the water content of the battery core is generally controlled below 200PPM before the liquid injection, and the battery bulge is caused due to a series of subsequent chain reactions caused by even trace water.
Detailed Description
The technical solution for achieving the object of the present invention will be further described with reference to several specific examples, but it should be noted that the technical solution claimed in the present invention includes but is not limited to the following examples.
Example 1
The embodiment discloses a lithium ion battery electrolyte, which comprises the following components:
the organic solvent accounts for 89.5% of the mass of the electrolyte, and the organic solvent is a mixture of dimethyl carbonate, diethyl carbonate, ethylmethyl carbonate and ethylene carbonate, wherein the mass of the dimethyl carbonate accounts for 12% of the mass of the electrolyte, the mass of the diethyl carbonate accounts for 30% of the mass of the electrolyte, the mass of the ethylmethyl carbonate accounts for 24% of the mass of the electrolyte, and the mass of the ethylene carbonate accounts for 23.5% of the mass of the electrolyte.
Heteropoly blue electrolyte salt with mass ratio of 10%, wherein the heteropolyblue electrolyte salt is polyacid H 3 PMo 12 O 40 Preparing 1 mol per liter of aqueous solution, preparing 0.5 mol per liter of aqueous solution of lithium sulfite, dropwise adding the lithium sulfite solution into the polyacid solution, oxidizing sulfite by the strong oxidizing property of the polyacid solution, reducing the polyacid into heteropolyblue, and simultaneously attracting lithium ions in the lithium sulfite by the strong negative charge of the heteropolyblue to form heteropolyblue lithium salt; after 4 hours of reaction, an electrolyte salt was obtained and dried at 40 degrees celsius for use.
The water-locking agent accounts for 0.5% of the mass of the water-locking agent, and is the mixture of polyvinylpyrrolidone (PVP) and PVP-K30.
The heteropolyblue electrolyte salt and the water-locking agent are dissolved in the organic solvent to form the electrolyte of the example 1, the electrolyte of the example 1 is applied to a lithium cobalt oxide battery, and the prepared lithium cobalt oxide battery is subjected to a cycle test.
Example 2
The embodiment discloses a lithium ion battery electrolyte, which comprises the following components:
88.5% of organic solvent: the organic solvent is a mixture of dimethyl carbonate, diethyl carbonate, methylethyl carbonate and propylene carbonate, wherein the mass ratio of the dimethyl carbonate in the prepared electrolyte is 22.5%, the mass ratio of the diethyl carbonate in the prepared electrolyte is 26%, the mass ratio of the methylethyl carbonate in the prepared electrolyte is 24%, and the mass ratio of the propylene carbonate in the prepared electrolyte is 16%.
Heteropoly blue electrolyte salt with mass ratio of 10%, and the heteropolyblue electrolyte salt is polyacid H 3 PMo 12 O 40 Preparing 1 mol per liter of aqueous solution, preparing 0.5 mol per liter of aqueous solution of lithium sulfite, dropwise adding the lithium sulfite solution into the polyacid solution, oxidizing sulfite by the strong oxidizing property of the polyacid solution, reducing the polyacid into heteropolyblue, and simultaneously attracting lithium ions in the lithium sulfite by the strong negative charge of the heteropolyblue to form heteropolyblue lithium salt; after 4 hours of reaction, an electrolyte salt was obtained and dried at 40 degrees celsius for use.
The water-locking agent accounts for 0.5% of the mass of the water-locking agent, and is the mixture of polyvinylpyrrolidone (PVP) and PVP-K30. The electrolyte salt and the water-blocking agent were dissolved in the organic solvent prepared in the above proportions to form the electrolyte of example 2.
The heteropolyblue electrolyte salt and the water-blocking agent are dissolved in the organic solvent to form the electrolyte of the example 2, the electrolyte of the example 2 is applied to a lithium cobalt oxide battery, and the prepared lithium cobalt oxide battery is subjected to a cycle test.
Example 3
The embodiment discloses a lithium ion battery electrolyte, which comprises the following components:
89.2% of organic solvent: the organic solvent is a mixture of dimethyl carbonate, diethyl carbonate, methylethyl carbonate and ethylene carbonate, wherein the mass ratio of the dimethyl carbonate in the prepared electrolyte is 42%, the mass ratio of the diethyl carbonate in the prepared electrolyte is 10%, the mass ratio of the methylethyl carbonate in the prepared electrolyte is 30%, and the mass ratio of the ethylene carbonate in the prepared electrolyte is 7.2%.
Heteropoly blue electrolyte salt with mass ratio of 10%, wherein the heteropolyblue electrolyte salt is polyacid H 3 PMo 12 O 40 Preparing 1 mol per liter of aqueous solution, preparing 0.5 mol per liter of aqueous solution of lithium sulfite, dropwise adding the lithium sulfite solution into the polyacid solution, oxidizing sulfite by the strong oxidizing property of the polyacid solution, reducing the polyacid into heteropolyblue, and simultaneously attracting lithium ions in the lithium sulfite by the strong negative charge of the heteropolyblue to form heteropolyblue lithium salt; after 4 hours of reaction, an electrolyte salt was obtained at 4Drying at 0 deg.c for use.
The water-locking agent accounts for 0.5% of the mass of the water-locking agent, and is the mixture of polyvinylpyrrolidone (PVP) and PVP-K30.
The heteropolyblue electrolyte salt and the water-blocking agent are dissolved in the organic solvent to form an electrolyte of example 3, the electrolyte of example 3 is applied to a lithium cobalt oxide battery, and the prepared lithium cobalt oxide battery is subjected to a cycle test.
Example 4
The embodiment discloses a lithium ion battery electrolyte, which comprises the following components:
the organic solvent accounts for 89.5% of the mass of the electrolyte, and the organic solvent is a mixture of dimethyl carbonate, diethyl carbonate, ethylmethyl carbonate and ethylene carbonate, wherein the mass of the dimethyl carbonate accounts for 12% of the mass of the electrolyte, the mass of the diethyl carbonate accounts for 30% of the mass of the electrolyte, the mass of the ethylmethyl carbonate accounts for 24% of the mass of the electrolyte, and the mass of the ethylene carbonate accounts for 23.5% of the mass of the electrolyte.
Heteropoly blue electrolyte salt with mass ratio of 10%, wherein the heteropolyblue electrolyte salt is polyacid H 3 PMo 12 O 40 Preparing 1 mol per liter of aqueous solution, preparing 0.5 mol per liter of aqueous solution of lithium sulfite, dropwise adding the lithium sulfite solution into the polyacid solution, oxidizing sulfite by the strong oxidizing property of the polyacid solution, reducing the polyacid into heteropolyblue, and simultaneously attracting lithium ions in the lithium sulfite by the strong negative charge of the heteropolyblue to form heteropolyblue lithium salt; after 4 hours of reaction, an electrolyte salt was obtained and dried at 40 degrees celsius for use.
The water-locking agent accounts for 0.5% of the mass of the water-locking agent, and is the mixture of polyvinylpyrrolidone (PVP) and PVP-K30.
The heteropolyblue electrolyte salt and the water-blocking agent are dissolved in the organic solvent to form the electrolyte of example 4, the electrolyte of example 4 is applied to a lithium cobalt oxide battery, and the prepared lithium cobalt oxide battery is subjected to a cycle test.
Comparative example 1
The lithium ion battery electrolyte disclosed in the comparative example comprises the following components:
the organic solvent accounts for 89.5% of the mass of the electrolyte, and the organic solvent is a mixture of dimethyl carbonate, diethyl carbonate, ethylmethyl carbonate and ethylene carbonate, wherein the mass of the dimethyl carbonate accounts for 12% of the mass of the electrolyte, the mass of the diethyl carbonate accounts for 30% of the mass of the electrolyte, the mass of the ethylmethyl carbonate accounts for 24% of the mass of the electrolyte, and the mass of the ethylene carbonate accounts for 23.5% of the mass of the electrolyte.
Electrolyte salt with the mass ratio of 10% adopts lithium hexafluorophosphate.
The water-locking agent accounts for 0.5% of the mass of the water-locking agent, and is the mixture of polyvinylpyrrolidone (PVP) and PVP-K30.
The electrolyte salt and the water-locking agent are dissolved in the organic solvent to form the electrolyte of the comparative example 1, the electrolyte of the comparative example 1 is applied to a lithium cobalt oxide battery, and the prepared lithium cobalt oxide battery is subjected to a cycle test.
Comparative example 2
The lithium ion battery electrolyte disclosed in the comparative example comprises the following components:
the organic solvent accounts for 89.5% of the mass of the electrolyte, and the organic solvent is a mixture of dimethyl carbonate, diethyl carbonate, ethylmethyl carbonate and ethylene carbonate, wherein the mass of the dimethyl carbonate accounts for 12% of the mass of the electrolyte, the mass of the diethyl carbonate accounts for 30% of the mass of the electrolyte, the mass of the ethylmethyl carbonate accounts for 24% of the mass of the electrolyte, and the mass of the ethylene carbonate accounts for 23.5% of the mass of the electrolyte.
Electrolyte salt with the mass ratio of 10% adopts lithium hexafluorophosphate.
The electrolyte salt was dissolved in the organic solvent to form an electrolyte of comparative example 2, the electrolyte of comparative example 2 was applied to a lithium cobaltate battery, and the prepared lithium cobaltate battery was subjected to a cycle test.
The test results are shown in table 1 below,
TABLE 1
。
As can be seen from table 1, the cycle life of the lithium cobaltate battery prepared by the electrolyte prepared by the method of the invention is obviously better than that of the lithium cobaltate battery using lithium hexafluorophosphate as electrolyte salt, and the cycle life of the lithium cobaltate battery using the water-locking agent is also better than that of the lithium cobaltate battery without the water-locking agent.

Claims (3)

1. The lithium ion battery electrolyte is characterized by comprising the following components:
the organic solvent accounts for 85-95% of the mass of the mixture, and the organic solvent is one or more of dimethyl carbonate, diethyl carbonate, ethylmethyl carbonate, propylene carbonate and ethylene carbonate;
the heteropolyblue electrolyte salt with the mass ratio of 10% -20% is Li 3 XY 12 O 40 Or Li (lithium) 4 XY 12 O 40 A lithium polyacid salt of a reduced structure, wherein X is a silicon element Si or a phosphorus element P, and Y is a tungsten element W or a molybdenum element Mo;
the water-locking agent accounts for 0% -2% of the mass, the water-locking agent is polyvinylpyrrolidone, and the polyvinylpyrrolidone comprises one or more of PVP-K12, PVP-K15, PVP-K17, PVP-K25, PVP-K30, PVP-K45, PVP-K60, PVP-K70, PVP-K80, PVP-K85, PVP-K90, PVP-K100, PVP-K110, PVP-K120 and PVP-K150;
the heteropolyblue electrolyte salt is prepared by mixing polyacid H 3 XY 12 O 40 Preparing 1 mol per liter of aqueous solution, and preparing 0.5 mol per liter of aqueous solution of lithium sulfite; and then the prepared lithium sulfite solution is dripped into a polyacid solution, so that the strong oxidizing property of the polyacid solution oxidizes sulfite, the polyacid is reduced into heteropolyblue, and meanwhile, lithium ions in the lithium sulfite are attracted by negative charges of the heteropolyblue to form the heteropolyblue electrolyte salt.
2. A lithium ion battery electrolyte as in claim 1, wherein: and (3) dropwise adding the prepared lithium sulfite solution into the polyacid solution to react for 4 hours to obtain the heteropolyblue electrolyte salt, and drying the obtained heteropolyblue electrolyte salt at the temperature of 40 ℃ for standby.
3. A lithium ion battery electrolyte as claimed in claim 1 or 2, characterized in that: the organic solvent, the heteropolyblue electrolyte salt and the water-locking agent are prepared in advance respectively, and then the heteropolyblue electrolyte salt and the water-locking agent are added into the organic solvent according to the respective mass ratio to form the lithium ion battery electrolyte.
CN202111305179.8A 2021-11-05 2021-11-05 Lithium ion battery electrolyte Active CN114221030B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102983362A (en) * 2012-12-20 2013-03-20 中国东方电气集团有限公司 Low-temperature electrolyte for LiFePO4 (lithium iron phosphate) lithium-ion batteries
CN108470897A (en) * 2018-03-26 2018-08-31 中国东方电气集团有限公司 A kind of preparation method of heteropoly blue lithium salts graphene negative material
CN110867613A (en) * 2019-11-19 2020-03-06 凌帕新能源科技(上海)有限公司 Silicon-carbon negative electrode lithium ion battery electrolyte and lithium battery
WO2021196429A1 (en) * 2020-03-31 2021-10-07 山东海容电源材料股份有限公司 High-voltage lithium ion battery electrolyte and preparation method therefor

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102983362A (en) * 2012-12-20 2013-03-20 中国东方电气集团有限公司 Low-temperature electrolyte for LiFePO4 (lithium iron phosphate) lithium-ion batteries
CN108470897A (en) * 2018-03-26 2018-08-31 中国东方电气集团有限公司 A kind of preparation method of heteropoly blue lithium salts graphene negative material
CN110867613A (en) * 2019-11-19 2020-03-06 凌帕新能源科技(上海)有限公司 Silicon-carbon negative electrode lithium ion battery electrolyte and lithium battery
WO2021196429A1 (en) * 2020-03-31 2021-10-07 山东海容电源材料股份有限公司 High-voltage lithium ion battery electrolyte and preparation method therefor

Non-Patent Citations (2)

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Title
Keggin结构合钒混配型杂多蓝的离析和性质研究;王作屏，任群翔，许林，沈恩洪，王恩波;无机化学学报(第01期);第63-67页 *
钴取代型钼硅杂多蓝稀土盐的合成及性质研究;刘杰, 王恩波, 王作屏, 胡长文;高等学校化学学报(第08期);第1200-1204页 *

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