CN110085915B - Lithium perchlorate electrolyte solution and preparation method thereof - Google Patents

Lithium perchlorate electrolyte solution and preparation method thereof Download PDF

Info

Publication number
CN110085915B
CN110085915B CN201910457866.8A CN201910457866A CN110085915B CN 110085915 B CN110085915 B CN 110085915B CN 201910457866 A CN201910457866 A CN 201910457866A CN 110085915 B CN110085915 B CN 110085915B
Authority
CN
China
Prior art keywords
lithium
electrolyte solution
lithium perchlorate
perchlorate
solvent
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910457866.8A
Other languages
Chinese (zh)
Other versions
CN110085915A (en
Inventor
李立飞
周玉梅
黄建
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu Langu New Energy Technology Co ltd
Original Assignee
Tianmu Lake Institute of Advanced Energy Storage Technologies Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tianmu Lake Institute of Advanced Energy Storage Technologies Co Ltd filed Critical Tianmu Lake Institute of Advanced Energy Storage Technologies Co Ltd
Priority to CN201910457866.8A priority Critical patent/CN110085915B/en
Publication of CN110085915A publication Critical patent/CN110085915A/en
Application granted granted Critical
Publication of CN110085915B publication Critical patent/CN110085915B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/052Li-accumulators
    • H01M10/0525Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/056Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564Accumulators 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
    • H01M10/0566Liquid materials
    • H01M10/0568Liquid materials characterised by the solutes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00Electrolytes
    • H01M2300/0017Non-aqueous electrolytes
    • H01M2300/0025Organic electrolyte
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention provides a preparation method of a lithium perchlorate electrolyte solution, which comprises the following steps: adding a lithium source and perchlorate into an organic solvent, heating for reaction, introducing inert gas to remove water in the solvent, filtering to remove salt byproducts insoluble in the solvent, and removing impurities and water in the filtrate by a molecular sieve to obtain the lithium perchlorate electrolyte solution. The preparation method of the lithium perchlorate electrolyte solution replaces the common water solution with the common ester or ether solvent of the electrolyte, reduces the solid drying process, removes the generated by-product by filtration when the generated by-product is not dissolved in the used ester or ether, generates no water in the reaction process, and has low water content of the final product by the water removal and various drying processes, and the product after filtration, drying and impurity removal can be directly prepared into the electrolyte subsequently.

Description

Lithium perchlorate electrolyte solution and preparation method thereof
Technical Field
The invention belongs to the field of lithium ion batteries, and particularly relates to a lithium perchlorate electrolyte solution and a preparation method thereof.
Background
With the continuous development of national economy, the required energy consumption is increased sharply, the development of clean energy is not slow enough, the clean energy represented by solar energy and tidal energy is greatly influenced by environmental factors, and the use of energy storage equipment can utilize the new energy more efficiently, so that the research and development of the energy storage equipment have great value, and lithium ion batteries are the most ideal energy storage equipment at present due to the advantages of large output power, high energy density, high working voltage, long cycle life and the like.
The electrolyte lithium salt is used as an important component of the lithium ion battery, not only plays a role in providing free shuttle transmission ions for the lithium ion battery, but also largely determines the capacity, the cycle performance, the power density, the energy density and other performances of the lithium ion battery.
Lithium perchlorate (LiClO)4) The lithium salt used as the lithium ion battery has high solubility, high ionic conductivity and wide electrochemical stability windowAnd good chemical stability.
The existing preparation methods of lithium perchlorate mainly comprise three methods: <1> neutralization method: reacting lithium carbonate or lithium hydroxide monohydrate with perchloric acid or ammonium perchlorate in pure water, evaporating and concentrating, cooling and crystallizing, centrifugally separating out perchloric acid trihydrate, dehydrating at high temperature, cooling and crushing to obtain the finished product. <2> double decomposition method: adding sodium perchlorate and lithium chloride into an aqueous solution, heating at 50 ℃ to perform double decomposition reaction, removing sodium chloride by-products by a low-temperature selective crystallization method, placing the solution at 0 ℃ to crystallize and separate out lithium perchlorate crystals, and heating and dehydrating to obtain the anhydrous lithium perchlorate. <3> electrolytic method: electrolyzing the lithium chlorate aqueous solution to prepare the lithium chlorate.
However, the neutralization method has the defects of high impurity content, high moisture content and the like, and the lithium carbonate neutralization method has the defects of long neutralization reaction time with perchloric acid, low speed, difficult filtration and the like due to low solubility of lithium carbonate. The double decomposition method has high sodium content and low product purity, and a low-temperature selective crystallization method is used for removing sodium chloride as a byproduct, so that the sodium chloride is difficult to completely remove. The electrolysis method has large energy consumption, large equipment investment and high cost.
Disclosure of Invention
In view of this, the invention aims to provide a lithium perchlorate electrolyte solution and a preparation method thereof, which are simpler and more convenient and have low cost.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a preparation method of a lithium perchlorate electrolyte solution comprises the following steps: adding a lithium source and perchlorate into an organic solvent, heating for reaction, introducing inert gas to remove water in the solvent, filtering to remove salt byproducts insoluble in the solvent, and removing impurities and water in the filtrate by a molecular sieve to obtain the lithium perchlorate electrolyte solution.
The lithium perchlorate obtained by the reaction is dissolved in an organic solvent, salt byproducts which are insoluble in the organic solvent are removed by filtration, the solvent volatilized in the evaporation process is recycled by a condensation recovery device, and the filtrate is subjected to secondary impurity removal by the processes until no salt byproducts are separated out. Finally, the mixed solution of the lithium perchlorate and the organic solvent is obtained and can be directly used for the preparation of the subsequent electrolyte.
Further, the organic solvent is at least one of ester or ether solvents; the ester solvent is one or a mixture of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, ethylene carbonate and propylene carbonate; the ether solvent is one or a mixture of tetrahydrofuran, 2-methyltetrahydrofuran, 1, 3-dioxolane, dimethoxymethane, 1, 2-dimethylethane and diglyme.
Further, the molecular sieve is one of 4A or 5A type molecular sieves.
Further, the organic solvent evaporated in the heating step is condensed and refluxed for recycling.
Further, the temperature of the heating step is 80-270 ℃, and the time is 5-24 h; preferably, the temperature of the heating step is 100-140 ℃.
Further, the lithium source is one or a mixture of more of lithium chloride, lithium carbonate, lithium bromide, lithium fluoride, lithium iodide, lithium argon, lithium carbide, lithium oxide and lithium hydride.
Further, the inert gas is argon.
Further, the mass fraction of the lithium perchlorate in the lithium perchlorate electrolyte solution is 5-70%.
Further, the mass ratio of the lithium source to the perchlorate is 1: 1.1-2; the mass ratio of the lithium source to the organic solvent is 1: 1.42-20.
A lithium perchlorate electrolyte solution is prepared from the following raw materials in parts by weight:
1 part of a lithium source;
1.1-2 parts of perchlorate;
1.42-20 parts of organic solvent.
Compared with the prior art, the preparation method of the perchlorate and the electrolyte solution thereof have the following advantages:
(1) the preparation method of the lithium perchlorate electrolyte solution replaces the common water solution with the common ester or ether solvent of the electrolyte, reduces the solid drying process, removes the generated by-product by filtration when the generated by-product is not dissolved in the used ester or ether, generates no water in the reaction process, and has low water content of the final product by the water removal and various drying processes, and the product after filtration, drying and impurity removal can be directly prepared into the electrolyte subsequently.
(2) The preparation method of the lithium perchlorate electrolyte solution does not use perchloric acid, lithium hydroxide and other raw materials with strong corrosivity and strong irritation, reduces the danger degree of the existing crystalline state method, and has simpler preparation method and low cost.
Detailed Description
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The test reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The present invention will be described in detail with reference to examples.
Example 1
A preparation method of a lithium perchlorate electrolyte solution comprises the following steps: adding 50g of lithium chloride and 80g of sodium perchlorate into a reaction kettle, then adding 182mL of ethylene glycol dimethyl ether solution, stirring for 3h at the reaction temperature of 100 ℃, introducing inert gas argon to remove excessive water, filtering to remove sodium chloride by-products insoluble in ethylene glycol dimethyl ether, returning the evaporated ethylene glycol dimethyl ether solution into the reaction kettle after reflux condensation, returning the filtrate into the reaction kettle again for secondary reaction until no precipitate is separated out, heating the obtained filtrate to 80 ℃, then cooling to 0 ℃ for filtering, removing sodium perchlorate which is not completely reacted, then filtering the filtrate by using a 4A molecular sieve, removing impurities and water in the solvent, and finally obtaining lithium perchlorate accounting for 30% of the mass of the ethylene glycol dimethyl ether solution, and testing the contents of water, impurities and the like in the solution by using a tester, wherein the product quality is shown in Table 1. In comparison with comparative example 1, the content of each impurity in the lithium perchlorate electrolyte solution prepared by the method is the same as that in the mixed solution of commercial pure lithium perchlorate and commercial glycol dimethyl ether, which shows that the lithium perchlorate electrolyte solution prepared by the method of the invention has high purity.
A lithium perchlorate electrolyte solution made from raw materials comprising by weight: 50g of lithium chloride, 80g of sodium perchlorate and 182mL of ethylene glycol dimethyl ether solution.
Example 2
A preparation method of a lithium perchlorate electrolyte solution comprises the following steps: adding 50g of lithium chloride and 80g of sodium perchlorate into a reaction kettle, then adding 182mL of diethyl carbonate solution, stirring for 3h at the reaction temperature of 140 ℃, introducing inert gas argon to remove excessive water, filtering to remove sodium chloride by-products insoluble in diethyl carbonate, returning evaporated diethyl carbonate solvent into the reaction kettle through reflux condensation, returning the filtrate into the reaction kettle again for secondary reaction until no precipitate is separated out, heating the obtained filtrate to 80 ℃, then cooling to 0 ℃ for filtering, removing sodium perchlorate which is not completely reacted, then filtering the filtrate through a 4A molecular sieve, removing impurities and water in the solvent, finally obtaining lithium perchlorate accounting for 35% by mass of the dimethyl carbonate solution, and testing the contents of water, impurities and the like in the solution by using a tester, wherein the product quality is shown in Table 1. Example 2 in comparison with comparative example 2, the lithium perchlorate electrolyte solution prepared by the method only has chlorate content and potassium ion content which are slightly higher than those of a mixed solution of commercially pure lithium perchlorate and commercially pure diethyl carbonate, which shows that the lithium perchlorate electrolyte solution prepared by the method of the invention still has higher purity, and compared with the results of example 1 and comparative example 1, the effect is slightly lower than that of example 1, which shows that the effect of diethyl carbonate is slightly reduced by replacing solvent ethylene glycol dimethyl ether, but the effect is still good.
A lithium perchlorate electrolyte solution made from raw materials comprising by weight: 50g of lithium chloride, 80g of sodium perchlorate and 182mL of diethyl carbonate solution.
Example 3
A preparation method of a lithium perchlorate electrolyte solution comprises the following steps: adding 60g of lithium bromide and 96g of sodium perchlorate into a reaction kettle, then adding 218mL of ethylene glycol dimethyl ether solution, stirring for 3h at the reaction temperature of 100 ℃, introducing inert gas argon to remove excessive moisture, reducing the temperature to 51 ℃, filtering to remove precipitated sodium bromide by-products, returning the evaporated ethylene glycol dimethyl ether solution into the reaction kettle through reflux condensation, returning the filtrate into the reaction kettle again for secondary reaction until no precipitate is precipitated, heating the obtained filtrate to 80 ℃, then cooling to 0 ℃ for filtering to remove sodium perchlorate which is not completely reacted, then filtering the filtrate through a 4A molecular sieve to remove impurities and moisture in the solvent, and finally testing the content of the lithium perchlorate in the ethylene glycol dimethyl ether solution by using a tester, wherein the product quality is shown in Table 1. In example 3, the lithium perchlorate electrolyte solution prepared by replacing lithium chloride with lithium bromide had a lower percentage of lithium salt than in example 1 and increased moisture and impurities than in comparative example 1, indicating that the lithium bromide used as the lithium source was not as effective as lithium chloride in this process.
A lithium perchlorate electrolyte solution made from raw materials comprising by weight: 60g of lithium bromide, 96g of sodium perchlorate and 218mL of ethylene glycol dimethyl ether solution.
Example 4
A preparation method of a lithium perchlorate electrolyte solution comprises the following steps: adding 80g of lithium chloride and 128g of sodium perchlorate into a reaction kettle, then adding 120mL of ethylene glycol dimethyl ether solution, stirring for 3h at the reaction temperature of 100 ℃, introducing inert gas argon to remove excessive water, filtering to remove sodium chloride by-products insoluble in ethylene glycol dimethyl ether, returning the evaporated ethylene glycol dimethyl ether solution into the reaction kettle after reflux condensation, returning the filtrate into the reaction kettle again for secondary reaction until no precipitate is separated out, heating the obtained filtrate to 80 ℃, then cooling to 0 ℃ for filtering, removing sodium perchlorate which is not completely reacted, then filtering the filtrate by using a 4A molecular sieve, removing impurities and water in the solvent, and finally obtaining lithium perchlorate accounting for 50% of the mass of the ethylene glycol dimethyl ether solution, and testing the contents of water, impurities and the like in the solution by using a tester, wherein the product quality is shown in Table 1. Example 4 increased the mass ratio of the lithium source to the organic solvent compared to example 1, and although the lithium perchlorate electrolyte solution was prepared with a high percentage of lithium salt, the moisture and the respective impurity contents were increased compared to comparative example 1, indicating that the mass ratio had a poor effect on the results in this method.
A lithium perchlorate electrolyte solution made from raw materials comprising by weight: 80g of lithium chloride, 128g of sodium perchlorate and 120mL of ethylene glycol dimethyl ether solution.
Example 5
A preparation method of a lithium perchlorate electrolyte solution comprises the following steps: adding 70g of lithium chloride and 112g of sodium perchlorate into a reaction kettle, adding 255mL of ethylene glycol dimethyl ether solution, stirring for 3h at the reaction temperature of 120 ℃, introducing inert gas argon to remove excessive water, filtering to remove sodium chloride by-products insoluble in ethylene glycol dimethyl ether, returning the evaporated ethylene glycol dimethyl ether solution into the reaction kettle after reflux condensation, returning the filtrate into the reaction kettle again for secondary reaction until no precipitate is separated out, heating the obtained filtrate to 80 ℃, cooling to 0 ℃ for filtering, removing sodium perchlorate which is not completely reacted, filtering the filtrate by using a 4A molecular sieve, removing impurities and water in the solvent, and finally obtaining lithium perchlorate accounting for 30% of the mass of the ethylene glycol dimethyl ether solution, and testing the contents of water, impurities and the like in the solution by using a tester, wherein the product quality is shown in Table 1. In example 5, the heating temperature was increased from 100 c to 120 c as compared with example 1, and the percentage content of lithium salt in the lithium perchlorate electrolyte solution was constant, and the content of each impurity was increased as compared with comparative example 1 although the moisture content was decreased, indicating that the use of increased temperature in this method only decreased the moisture content, adversely affecting the other impurities.
A lithium perchlorate electrolyte solution made from raw materials comprising by weight: 70g of lithium chloride, 112g of sodium perchlorate and 255mL of ethylene glycol dimethyl ether solution.
Example 6
A preparation method of a lithium perchlorate electrolyte solution comprises the following steps: adding 70g of lithium chloride and 112g of sodium perchlorate into a reaction kettle, adding 255mL of ethylene glycol dimethyl ether solution, stirring for 10h at the reaction temperature of 100 ℃, introducing inert gas argon to remove excessive water, filtering to remove sodium chloride by-products insoluble in ethylene glycol dimethyl ether, returning the evaporated ethylene glycol dimethyl ether solvent into the reaction kettle through reflux condensation, returning the filtrate into the reaction kettle again to perform secondary reaction until no precipitate is separated out, heating the obtained filtrate to 80 ℃, cooling to 0 ℃ to filter, removing sodium perchlorate which is not completely reacted, filtering the filtrate through a 4A molecular sieve to remove impurities and water in the solvent, and finally obtaining lithium perchlorate accounting for 35% by mass of the ethylene glycol dimethyl ether solution, and testing the contents of water, impurities and the like in the solution by using a tester, wherein the product quality is shown in Table 1. Example 6 extended the reaction time to make the reaction more complete, increased the percentage content of lithium salt in the prepared lithium perchlorate electrolyte solution, slightly increased the moisture content, potassium element content, sodium element content and lead element content, and slightly decreased the content of other impurities, compared to comparative example 1, indicating that extension of the reaction time in this method had a good effect only on a portion of the impurities.
A lithium perchlorate electrolyte solution made from raw materials comprising by weight: 70g of lithium chloride, 112g of sodium perchlorate and 255mL of ethylene glycol dimethyl ether solution.
Example 7
A preparation method of a lithium perchlorate electrolyte solution comprises the following steps: adding 50g of lithium chloride and 100g of sodium perchlorate into a reaction kettle, then adding 182mL of ethylene glycol dimethyl ether solution, stirring for 3h at the reaction temperature of 100 ℃, introducing inert gas argon to remove excessive water, filtering to remove sodium chloride by-products insoluble in ethylene glycol dimethyl ether, returning the evaporated ethylene glycol dimethyl ether solution into the reaction kettle after reflux condensation, returning the filtrate into the reaction kettle again for secondary reaction until no precipitate is separated out, heating the obtained filtrate to 80 ℃, then cooling to 0 ℃ for filtering, removing sodium perchlorate which is not completely reacted, then filtering the filtrate by using a 4A molecular sieve, removing impurities and water in the solvent, and finally obtaining lithium perchlorate accounting for 30% of the mass of the ethylene glycol dimethyl ether solution, and testing the contents of water, impurities and the like in the solution by using a tester, wherein the product quality is shown in Table 1. Compared with the comparative example 1, in the example 7, the content of perchlorate is increased, the mass ratio of the lithium source to the perchlorate is improved, the percentage content of lithium salt in the prepared lithium perchlorate electrolyte solution is unchanged, compared with the comparative example 1, the chlorate content and the sodium element content are obviously increased, and the others are slightly increased, which indicates that the amount of perchlorate is increased, and the difficulty in removing redundant perchlorate and the difficulty in removing byproducts are increased.
A lithium perchlorate electrolyte solution made from raw materials comprising by weight: 50g of lithium chloride, 100g of sodium perchlorate and 182mL of ethylene glycol dimethyl ether solution.
Comparative example 1
A preparation method of a lithium perchlorate electrolyte solution comprises the following steps: commercial lithium perchlorate and commercial ethylene glycol dimethyl ether are mixed to prepare a mixed electrolyte with the mass percentage of the lithium perchlorate of 30 percent, and a tester is used for testing the contents of moisture, impurities and the like in the solution, which is shown in table 1.
Comparative example 2
A preparation method of a lithium perchlorate electrolyte solution comprises the following steps: commercial lithium perchlorate and commercial dimethyl carbonate are mixed to prepare a mixed electrolyte with the mass percentage of the lithium perchlorate of 35 percent, and a tester is used for testing the contents of moisture, impurities and the like in the solution, which is shown in table 1.
Note: in all the above examples, the content of each impurity is lower than the national standard for the content of each impurity in lithium perchlorate.
The test results of the lithium perchlorate electrolyte solutions obtained in examples 1 to 7 and comparative examples 1 to 2 are shown in the following tables.
TABLE 1 test results of lithium perchlorate electrolyte solutions obtained in examples 1 to 7 and comparative examples 1 to 2
Figure BDA0002077147750000091
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (9)

1. A preparation method of lithium perchlorate electrolyte solution is characterized by comprising the following steps: the method comprises the following steps: adding a lithium source and perchlorate into an organic solvent, heating for reaction, introducing inert gas to remove water in the solvent, filtering to remove salt byproducts insoluble in the solvent, and removing impurities and water in the filtrate by a molecular sieve to obtain the lithium perchlorate electrolyte solution; the lithium source is one or a mixture of more of lithium chloride, lithium bromide, lithium fluoride and lithium iodide; the organic solvent is at least one of ester or ether solvents; the ester solvent is one or a mixture of dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, ethylene carbonate and propylene carbonate; the ether solvent is one or a mixture of tetrahydrofuran, 2-methyltetrahydrofuran, 1, 3-dioxolane, dimethoxymethane, 1, 2-dimethylethane and diglyme.
2. The method for preparing a lithium perchlorate electrolyte solution according to claim 1, characterized in that: the molecular sieve is one of 4A or 5A type molecular sieves.
3. The method for preparing a lithium perchlorate electrolyte solution according to claim 1, characterized in that: the organic solvent evaporated in the heating step is condensed and refluxed for recycling.
4. The method for preparing a lithium perchlorate electrolyte solution according to claim 1, characterized in that: the temperature of the heating step is 80-270 ℃, and the time is 5-24 h.
5. The method for preparing a lithium perchlorate electrolyte solution according to claim 4, characterized in that: the temperature of the heating step is 100-140 ℃.
6. The method for preparing a lithium perchlorate electrolyte solution according to claim 1, characterized in that: the inert gas is argon.
7. The method for preparing a lithium perchlorate electrolyte solution according to claim 1, characterized in that: the mass fraction of the lithium perchlorate in the lithium perchlorate electrolyte solution is 5-70%.
8. The method for preparing a lithium perchlorate electrolyte solution according to claim 1, characterized in that: the mass ratio of the lithium source to the perchlorate is 1: 1.1-2; the mass ratio of the lithium source to the organic solvent is 1: 1.42-20.
9. A lithium perchlorate electrolyte solution prepared by the preparation method according to claim 1, characterized in that: the lithium perchlorate electrolyte solution is prepared from the following raw materials in parts by weight:
1 part of a lithium source;
1.1-2 parts of perchlorate;
1.42-20 parts of organic solvent.
CN201910457866.8A 2019-05-29 2019-05-29 Lithium perchlorate electrolyte solution and preparation method thereof Active CN110085915B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910457866.8A CN110085915B (en) 2019-05-29 2019-05-29 Lithium perchlorate electrolyte solution and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910457866.8A CN110085915B (en) 2019-05-29 2019-05-29 Lithium perchlorate electrolyte solution and preparation method thereof

Publications (2)

Publication Number Publication Date
CN110085915A CN110085915A (en) 2019-08-02
CN110085915B true CN110085915B (en) 2021-01-08

Family

ID=67422434

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910457866.8A Active CN110085915B (en) 2019-05-29 2019-05-29 Lithium perchlorate electrolyte solution and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110085915B (en)

Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2929680A (en) * 1957-06-28 1960-03-22 American Potash & Chem Corp Preparation of lithium perchlorate
US4065550A (en) * 1977-01-31 1977-12-27 The United States Of America As Represented By The Secretary Of The Army Process for preparing lithium hexafluoroarsenate of high purity
JPS611369B2 (en) * 1978-07-19 1986-01-16 Showa Denko Kk
JPS62192593A (en) * 1986-02-17 1987-08-24 Agency Of Ind Science & Technol Production of indium (iii) oxide
CN101233077A (en) * 2005-07-06 2008-07-30 贝洛赫尔有限公司 Solid salt preparation, the production thereof and its use
CN101819882A (en) * 2010-04-19 2010-09-01 中国科学院长春应用化学研究所 Electrolyte for super-capacitor and super-capacitor
CN102139861A (en) * 2011-05-10 2011-08-03 湖北百杰瑞新材料有限公司 Method for producing anhydrous lithium perchlorate
CN103367791A (en) * 2013-07-15 2013-10-23 中国科学院化学研究所 Novel lithium ion battery
CN103490071A (en) * 2013-09-23 2014-01-01 威海文隆电池有限公司 Lithium-polyaniline secondary battery and preparation method thereof
CN103700820A (en) * 2014-01-07 2014-04-02 中国科学院化学研究所 Lithium ion selenium battery with long service life
WO2014093978A1 (en) * 2012-12-14 2014-06-19 The Penn State Research Foundation Liquid electrolyte for increasing capacity and cycling retention of lithium sulfur battery
CN103943376A (en) * 2013-01-22 2014-07-23 中国科学院大连化学物理研究所 Electrolyte of mixed type super capacitor
CN106025307A (en) * 2016-07-22 2016-10-12 惠州市惠德瑞锂电科技股份有限公司 Lithium battery electrolyte and obtained lithium primary battery
CN106257714A (en) * 2015-12-21 2016-12-28 上海卡耐新能源有限公司 A kind of new system lithium ion battery and preparation method thereof
CN108698050A (en) * 2016-02-17 2018-10-23 纳米技术仪器公司 Produce the electrochemical method of single layer or few layer graphene piece

Patent Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2929680A (en) * 1957-06-28 1960-03-22 American Potash & Chem Corp Preparation of lithium perchlorate
US4065550A (en) * 1977-01-31 1977-12-27 The United States Of America As Represented By The Secretary Of The Army Process for preparing lithium hexafluoroarsenate of high purity
JPS611369B2 (en) * 1978-07-19 1986-01-16 Showa Denko Kk
JPS62192593A (en) * 1986-02-17 1987-08-24 Agency Of Ind Science & Technol Production of indium (iii) oxide
CN101233077A (en) * 2005-07-06 2008-07-30 贝洛赫尔有限公司 Solid salt preparation, the production thereof and its use
CN101819882A (en) * 2010-04-19 2010-09-01 中国科学院长春应用化学研究所 Electrolyte for super-capacitor and super-capacitor
CN102139861A (en) * 2011-05-10 2011-08-03 湖北百杰瑞新材料有限公司 Method for producing anhydrous lithium perchlorate
WO2014093978A1 (en) * 2012-12-14 2014-06-19 The Penn State Research Foundation Liquid electrolyte for increasing capacity and cycling retention of lithium sulfur battery
CN103943376A (en) * 2013-01-22 2014-07-23 中国科学院大连化学物理研究所 Electrolyte of mixed type super capacitor
CN103367791A (en) * 2013-07-15 2013-10-23 中国科学院化学研究所 Novel lithium ion battery
CN103490071A (en) * 2013-09-23 2014-01-01 威海文隆电池有限公司 Lithium-polyaniline secondary battery and preparation method thereof
CN103700820A (en) * 2014-01-07 2014-04-02 中国科学院化学研究所 Lithium ion selenium battery with long service life
CN106257714A (en) * 2015-12-21 2016-12-28 上海卡耐新能源有限公司 A kind of new system lithium ion battery and preparation method thereof
CN108698050A (en) * 2016-02-17 2018-10-23 纳米技术仪器公司 Produce the electrochemical method of single layer or few layer graphene piece
CN106025307A (en) * 2016-07-22 2016-10-12 惠州市惠德瑞锂电科技股份有限公司 Lithium battery electrolyte and obtained lithium primary battery

Also Published As

Publication number Publication date
CN110085915A (en) 2019-08-02

Similar Documents

Publication Publication Date Title
CN102803142A (en) Method for producing tetrafluoroborate
WO2023202093A1 (en) Preparation method for lithium bis(fluorosulfonyl)imide, and lithium ion battery
CN103265002A (en) Preparation method of lithium hexafluorophosphate
CN105859760A (en) A synthetic method of electronic grade lithium difluoro(oxalato)borate
KR20200114962A (en) Method for producing bis (fluorosulfonyl) imide lithium salt (LiFSI) with reduced fluorine anion content
CN114524422A (en) Preparation method of lithium bis (fluorosulfonyl) imide
JPS5981870A (en) Manufacture of solute for nonaqueous electrolyte
CN112897494B (en) Synthesis process and synthesis device of lithium difluorophosphate
KR20200114963A (en) Method for producing bis (fluorosulfonyl) imide lithium salt (LiFSI) with reduced fluorine anion content
CN113929711A (en) Preparation method of lithium difluoroborate
JPS5981869A (en) Manufacture of lithium battery
CN110085915B (en) Lithium perchlorate electrolyte solution and preparation method thereof
CN110683564B (en) Lithium hexafluorophosphate-containing mixture crystal and application thereof
CN101209830A (en) Method for preparing lithium hexafluorophosphate
KR20200114967A (en) Method for producing bis (fluorosulfonyl) imide lithium salt (LiFSI) with reduced fluorine anion content
CN116143666A (en) Preparation method of lithium ethylenesulfonic acid difluorophosphate triethylamine salt (1:1:1)
CN116040641A (en) Preparation method of lithium tetrafluoroborate
CN114573006B (en) Method for purifying and recovering lithium by-product lithium-containing crude sodium sulfate in lithium extraction process of nickel cobalt lithium manganate anode material recovery
CN115304039A (en) Purification device and method for bis (chlorosulfonyl) imide
JPS5953216B2 (en) Synthesis method of anhydrous lithium borofluoride
JPH11157830A (en) Production of lithium tetrafluoroborate
CN114368733A (en) Lithium bis (fluorosulfonyl) imide, preparation method thereof, electrolyte and secondary battery
CN114031053A (en) Preparation method of bis (fluorosulfonyl) imide salt
CN109369474B (en) Preparation method of lithium bis (trifluoromethylsulfonyl) imide
KR101982603B1 (en) Method for producing bis (fluorosulfonyl) imide lithium salt (LiFSI) with reduced fluorine anion content (2)

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20221109

Address after: 213300 room 808, building 1, No. 168, Xingcheng West Road, Bieqiao Town, Liyang City, Changzhou City, Jiangsu Province

Patentee after: Jiangsu langu New Energy Technology Co.,Ltd.

Address before: Room 327, building C, no.218, Hongkou Road, Kunlun Street, Liyang City, Changzhou City, Jiangsu Province

Patentee before: TIANMU LAKE INSTITUTE OF ADVANCED ENERGY STORAGE TECHNOLOGIES Co.,Ltd.