CN115196646A - Method for synthesizing lithium tetrafluoroborate - Google Patents
Method for synthesizing lithium tetrafluoroborate Download PDFInfo
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- CN115196646A CN115196646A CN202211013816.9A CN202211013816A CN115196646A CN 115196646 A CN115196646 A CN 115196646A CN 202211013816 A CN202211013816 A CN 202211013816A CN 115196646 A CN115196646 A CN 115196646A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
- C01B35/063—Tetrafluoboric acid; Salts thereof
- C01B35/066—Alkali metal tetrafluoborates
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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
- H01M10/052—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
- 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
- H01M10/0567—Liquid materials characterised by the additives
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a method for synthesizing lithium tetrafluoroborate, which comprises the following steps: (1) Adding boric acid into aqueous hydrogen fluoride under the protection of inert gas to prepare aqueous tetrafluoroborate; (2) Dispersing a high-purity lithium source in a carbonate solution to prepare a carbonate suspension of the lithium source: (3) And (3) at low temperature, dropwise adding the tetrafluoroborate aqueous solution into a carbonate solution of a lithium source, separating to obtain an organic phase, and concentrating, crystallizing, filtering and drying to obtain a pure lithium tetrafluoroborate product. The invention has the advantages of simple and easily obtained raw materials, simple production process, high yield and low cost, and is suitable for large-scale production and application.
Description
Technical Field
The invention relates to a synthesis method of an electrolyte additive of a lithium ion battery, in particular to a synthesis method of lithium tetrafluoroborate.
Background
The lithium ion battery has small volume, large energy density, high working voltage and low self-discharge rate, is widely applied to the fields of power batteries, mobile communication and the like, and the electrolyte is an important component of the lithium ion battery and is a key for conveying ions between a positive electrode and a negative electrode so as to realize current conduction. The electrolyte additive with good performance is the key to improve the energy density and the power density of the battery, prolong the cycle life and improve the safety performance. The lithium tetrafluoroborate has good chemical stability and thermal stability, is insensitive to moisture, can improve the cycle life of the battery, broadens the working temperature range of the lithium ion battery, and improves the high-low temperature discharge performance of the battery.
The current common production method of lithium tetrafluoroborate comprises the following steps:
CN201910354134.6 discloses a preparation method of lithium tetrafluoroborate crystal particles, which comprises the steps of firstly preparing boron trifluoride, and then reacting with lithium fluoride to prepare lithium tetrafluoroborate, wherein in the process, the boron trifluoride is a gas at normal temperature, the reaction yield is low, and the requirement on equipment is high;
CN201811247879.4 discloses a preparation method of lithium tetrafluoroborate, which comprises the steps of preparing an aqueous solution of tetrafluoroborate by reacting hydrofluoric acid with boric acid, then reacting with lithium carbonate in water to prepare lithium tetrafluoroborate, and obtaining a target product by concentration, crystallization and recrystallization.
Disclosure of Invention
The invention aims to provide a preparation method of lithium hexafluorophosphate, which simplifies the preparation process flow, improves the yield and safety, and reduces the equipment requirement and the generation amount of three wastes.
In order to solve the technical problems, the invention provides the following technical scheme: a method for synthesizing lithium tetrafluoroborate comprises the following steps:
s1, preparing a synthetic liquid: under the protection of inert gas, adding hydrogen fluoride and boric acid into a reactor to react to obtain a tetrafluoroborate aqueous solution;
s2, preparing a carbonate suspension: dispersing a lithium source into carbonate to prepare carbonate suspension of the lithium source;
s3, preparing a lithium tetrafluoroborate solution: dropwise adding the tetrafluoroborate aqueous solution obtained in the step S1 into the carbonate suspension of the lithium source obtained in the step S2 to perform a synthesis reaction to obtain a tetrafluoroborate solution;
s4, concentrating and crystallizing: filtering insoluble substances from the lithium tetrafluoroborate solution, carrying out liquid separation treatment to obtain an organic phase, and carrying out concentration crystallization, filtration and drying on the organic phase to obtain solid lithium tetrafluoroborate;
s5, recycling: and (5) condensing carbonate vapor generated in the concentration process in the step (S4) to obtain carbonate liquid, and mechanically applying mother liquor obtained after crystallization and filtration to the step (S2) for preparing the lithium source dispersion liquid.
As a preferable scheme of the invention, in the step S1, stirring is required to be carried out firstly, then hydrogen fluoride is added into the reactor, and the temperature of the system is controlled to be-5 to 0 ℃ in the reaction process.
In a preferred embodiment of the present invention, in the step S2, a temperature environment when the lithium source is dispersed in the carbonate is between 10 ℃ and 30 ℃, the lithium source is lithium carbonate or lithium hydroxide, and the carbonate is dimethyl carbonate, diethyl carbonate or ethyl methyl carbonate.
In a preferred embodiment of the invention, in the step S3, the carbonate solution of the lithium source is placed in a closed container, the stirring is started under the condition that the temperature is controlled to be-5 to 0 ℃, and then the aqueous tetrafluoroborate solution is dropwise added.
As a preferable scheme of the invention, the temperature of the system is controlled to be not more than 0 ℃ in the process of dripping the tetrafluoroboric acid aqueous solution, and the dripping time is 5 to 7 hours.
In a preferred embodiment of the present invention, in step S4, the lithium tetrafluoroborate solution is subjected to suction filtration after the synthesis reaction is completed, insoluble substances are removed by suction filtration, then liquid separation treatment is performed, and the organic phase obtained by liquid separation is subjected to vacuum concentration and crystallization at 30 to 50 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the synthesis process route is simple and controllable, safe and efficient, no gas intermediate is generated, the requirement on equipment is low, the equipment investment is low, byproducts are few, and the synthesis yield of the lithium tetrafluoroborate is improved;
the high-purity lithium tetrafluoroborate product is obtained through concentration and crystallization, the purity can reach more than 99.9 percent, the product meets the standard of lithium ion battery electrolyte, and the concentrated and condensed carbonate solution and the crystallization mother solution are recycled, so that the cost is further reduced.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The embodiment of the invention provides a method for synthesizing lithium tetrafluoroborate, which comprises the following steps: under the protection of inert gas, setting the temperature between-5 ℃ and 0 ℃, opening and stirring, and then adding hydrogen fluoride and boric acid into a reactor for reaction to obtain a tetrafluoroborate aqueous solution;
dispersing a lithium source into carbonate at the temperature of 10-30 ℃ to prepare carbonate suspension of the lithium source, wherein the lithium source is preferably lithium carbonate or lithium hydroxide, and the carbonate is preferably dimethyl carbonate, diethyl carbonate or ethyl methyl carbonate;
putting a lithium source carbonate solution into a closed container, controlling the temperature to be-5 to 0 ℃, starting stirring, then dropwise adding a tetrafluoroboric acid aqueous solution to perform a synthetic reaction to obtain a tetrafluoroboric acid lithium solution, wherein the temperature of a control system in the process of dropwise adding the tetrafluoroboric acid aqueous solution is not more than 0 ℃, and the dropwise adding time is 5 to 7 hours;
and after the synthesis reaction is finished, carrying out suction filtration on the lithium tetrafluoroborate solution, carrying out liquid separation treatment after insoluble substances are removed by suction filtration, and carrying out reduced pressure concentration crystallization and drying on an organic phase obtained by liquid separation at 30-50 ℃ to obtain solid lithium tetrafluoroborate.
And (3) condensing carbonate steam generated in the concentration process to obtain carbonate liquid, and sleeving the crystallized and filtered mother liquor to the lithium source dispersion liquid for recycling.
Example 1
A reactor with stirring, jacket refrigeration and reflux is prepared, 1800.8g50% aqueous hydrogen fluoride solution is added, after the temperature is reduced to-5 ℃, 696g of boric acid is added in batches under stirring, the process control temperature is lower than 0 ℃, the feeding is finished within 3 hours, and the stirring is continued for 3 hours. 415.8g of lithium carbonate were dispersed in 3000g of dimethyl carbonate at room temperature. And (3) dropwise adding the tetrafluoroboric acid aqueous solution into a dimethyl carbonate suspension of lithium carbonate at the temperature of-5 to 0 ℃, controlling the temperature of the reaction system to be lower than 0 ℃ in the dropwise adding process, and ending the dropwise adding within 6.5 hours. Filtering and separating to obtain an organic phase, evaporating most of solvent in the organic phase under reduced pressure, cooling and crystallizing, filtering and drying to obtain 934.7g of lithium tetrafluoroborate solid with the content of 99.94 percent, the content of free acid (calculated by HF) of 87ppm, the content of moisture (Karl Fischer method) of 8ppm, the content of metal ions of 3ppm and the yield of 95.53 percent.
Example 2
A reactor with stirring, jacket refrigeration and reflux is prepared, 1851.4g of 50% aqueous hydrogen fluoride solution is added, the temperature is reduced to-5 ℃, 715.5g of boric acid is added in batches under stirring, the process control temperature is lower than 0 ℃, the feeding is finished after 3 hours, and the stirring is continued for 3 hours. 277.1g of lithium hydroxide were dispersed in 3000g of dimethyl carbonate at room temperature. And (3) dropwise adding the tetrafluoroborate aqueous solution into the lithium hydroxide dimethyl carbonate suspension at the temperature of-5 to 0 ℃, controlling the temperature of the reaction system to be lower than 0 ℃ in the dropwise adding process, and ending the dropwise adding within 6 hours. Filtering and separating to obtain an organic phase, evaporating most of solvent in the organic phase under reduced pressure, cooling and crystallizing, filtering and drying to obtain 944.6g of lithium tetrafluoroborate solid with the content of 99.95 percent, 82ppm of free acid (calculated by HF), 6ppm of moisture (Karl Fischer method), 3ppm of alkali metal ion content and the yield of 94.04 percent.
Example 3
A reactor with stirring, jacket refrigeration and reflux was prepared, 1823.6g of 50% aqueous hydrogen fluoride were added, the temperature was reduced to-5 ℃ and 704.7g of boric acid were added in portions with stirring, the process temperature was controlled below 0 ℃ and the addition was completed for 3 hours, and stirring was continued for 3 hours. After 1500g of recovered dimethyl carbonate and 1500g of recovered mother liquor of crystallization were uniformly mixed, 272.9g of lithium hydroxide was dispersed in the above mixed solution. And (3) dropwise adding the tetrafluoroboric acid aqueous solution into a dimethyl carbonate suspension of lithium hydroxide at the temperature of-5 to 0 ℃, controlling the temperature of a reaction system to be lower than 0 ℃ in the dropwise adding process, and ending the dropwise adding within 6.5 hours. Filtering and separating to obtain an organic phase, decompressing and steaming out most of the solvent in the organic phase, reducing the temperature and crystallizing, filtering and drying to obtain 942.3g of lithium tetrafluoroborate solid with the content of 99.92 percent, 74ppm of free acid (calculated by HF), 8ppm of moisture (Karl Fischer method), 3ppm of alkali metal ion content and the yield of 95.11 percent.
Example 4
A reactor with stirring, jacket refrigeration and reflux was prepared, 1890.6g of 50% aqueous hydrogen fluoride was added, the temperature was reduced to-5 deg.C, 730.6g of boric acid was added in portions with stirring, the process temperature was controlled below 0 deg.C, the addition was completed within 3.5 hours, and stirring was continued for 3 hours. After 1500g of recovered dimethyl carbonate and 1500g of recovered mother liquor for crystallization were uniformly mixed, 436.6g of lithium carbonate was dispersed in the above mixed solution. And (3) dropwise adding the tetrafluoroboric acid aqueous solution into a dimethyl carbonate suspension of lithium carbonate at the temperature of-5 to 0 ℃, controlling the temperature of the reaction system to be lower than 0 ℃ in the dropwise adding process, and ending the dropwise adding within 6.5 hours. Filtering and separating the solution to obtain an organic phase, decompressing and steaming out most of the solvent in the organic phase, reducing the temperature and crystallizing, filtering and drying to obtain 988.6g of lithium tetrafluoroborate solid with the content of 99.92 percent, 77ppm of free acid (calculated by HF), 6ppm of moisture (Karl Fischer method), 3ppm of alkali metal ion content and the yield of 96.18 percent.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (6)
1. A method for synthesizing lithium tetrafluoroborate is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing a synthetic liquid: under the protection of inert gas, adding hydrogen fluoride and boric acid into a reactor to react to obtain a tetrafluoroboric acid aqueous solution;
s2, preparing a carbonate suspension: dispersing a lithium source into carbonate to prepare carbonate suspension of the lithium source;
s3, preparing a lithium tetrafluoroborate solution: dropwise adding the tetrafluoroborate aqueous solution obtained in the step S1 into the carbonate suspension of the lithium source obtained in the step S2 for synthesis reaction to obtain a tetrafluoroborate lithium solution;
s4, concentrating and crystallizing: filtering insoluble substances from the lithium tetrafluoroborate solution, carrying out liquid separation treatment to obtain an organic phase, and carrying out concentration crystallization, filtration and drying on the organic phase to obtain solid lithium tetrafluoroborate;
s5, recycling: and (5) condensing carbonate vapor generated in the concentration process in the step (S4) to obtain carbonate liquid, and mechanically applying mother liquor obtained after crystallization and filtration to the step (S2) for preparing the lithium source dispersion liquid.
2. The method for synthesizing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: in the step S1, stirring is carried out firstly, then hydrogen fluoride is added into the reactor, and the temperature of the system is controlled to be-5 to 0 ℃ in the reaction process.
3. The method for synthesizing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: in the step S2, the temperature environment when the lithium source is dispersed into the carbonate is 10-30 ℃, the lithium source is lithium carbonate or lithium hydroxide, and the carbonate is dimethyl carbonate, diethyl carbonate or ethyl methyl carbonate.
4. The method for synthesizing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: and (3) putting the carbonate solution of the lithium source into a closed container, controlling the temperature to be within-5 to 0 ℃, starting stirring, and then dropwise adding the tetrafluoroborate aqueous solution.
5. The method for synthesizing lithium tetrafluoroborate according to claim 4, wherein the method comprises the following steps: the temperature of the system is controlled to be not more than 0 ℃ in the process of dripping the tetrafluoroboric acid aqueous solution, and the dripping time is 5 to 7 hours.
6. The method for synthesizing lithium tetrafluoroborate according to claim 1, wherein the method comprises the following steps: in the step S4, after the synthesis reaction is finished, the lithium tetrafluoroborate solution is subjected to suction filtration, insoluble substances are removed through suction filtration, then liquid separation treatment is performed, and an organic phase obtained through liquid separation is subjected to reduced pressure concentration and crystallization at 30-50 ℃.
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Citations (11)
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| JPH11157830A (en) * | 1997-11-19 | 1999-06-15 | Central Glass Co Ltd | Production of lithium tetrafluoroborate |
| US20060040180A1 (en) * | 2004-08-23 | 2006-02-23 | Ivanov Sergei V | High purity lithium polyhalogenated boron cluster salts useful in lithium batteries |
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| US20170197834A1 (en) * | 2014-07-31 | 2017-07-13 | Kanto Denka Kogyo Co., Ltd. | Method for producing difluorophospate |
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| CN109264736A (en) * | 2018-11-14 | 2019-01-25 | 东营石大胜华新能源有限公司 | A kind of preparation method of LiBF4 |
| FR3077415A1 (en) * | 2018-01-29 | 2019-08-02 | Arkema France | MIXTURE OF LITHIUM AND POTASSIUM SALTS AND USE THEREOF IN A BATTERY |
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2022
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Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11157830A (en) * | 1997-11-19 | 1999-06-15 | Central Glass Co Ltd | Production of lithium tetrafluoroborate |
| US20060040180A1 (en) * | 2004-08-23 | 2006-02-23 | Ivanov Sergei V | High purity lithium polyhalogenated boron cluster salts useful in lithium batteries |
| JP2009155130A (en) * | 2007-12-25 | 2009-07-16 | Stella Chemifa Corp | Method for producing tetrafluoroborate |
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