A kind of preparation method of difluorooxalate lithium borate electrolyte salt

A technology of lithium difluorooxalate borate and electrolyte salt, applied in secondary batteries, chemical instruments and methods, circuits, etc., can solve the problems of large SEI film resistance, high investment cost, staff health and environmental hazards, etc. Simple process, low corrosiveness, environment-friendly effect

Inactive Publication Date: 2011-11-30
CHANGZHOU GUOYA NEW ENERGY TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Lithium tetrafluoroborate (LiBF 4 ) relative to LiPF 6 Insensitive to environmental moisture, low charge transfer resistance at low temperature, so low temperature performance is better than LiPF 6 , but used alone will lead to a decrease in the capacity and coulombic efficiency of lithium-ion batteries; lithium bisoxalate borate (LiBOB) has good thermal stability and good electrochemical stability, and can form a stable and dense SEI film on graphite. The cycle performance of the battery is improved, but it is almost insoluble in some solvents with low dielectric constants (especially linear carbonates), and the formed SEI film has high resistance, poor low-temperature performance, and its application is limited.
Therefore, the shortcomings of this method are: (1) harm to the health of the staff and the environment, (2) high requirements for the corrosion resistance of the equipment, (3) high investment costs

Method used

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  • A kind of preparation method of difluorooxalate lithium borate electrolyte salt

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Lithium difluorooxalate borate was prepared by using lithium fluoride, boric acid and oxalic acid as raw materials.

[0024] Step 1: Put 30.9 g of boric acid and 26 g of lithium fluoride into a ball mill jar, mix and ball mill for 12 hours at 5° C., and the speed of the planetary ball mill is 380 rpm.

[0025] Step 2: Put the ball-milled raw materials above in a muffle furnace, raise the temperature to 350° C. under the protection of nitrogen, and keep the temperature constant for 20 hours to make them react completely.

[0026] Step 3. Transfer the above-mentioned treated raw materials to an appropriate amount of water, stir while heating, and then add 94.8 g of oxalic acid after the mixture is evenly mixed. After the reaction is complete, put the solution into a blast drying oven to remove water to obtain a white product.

[0027] Step 4. Grind the white product finely, then put it into a container, add 1500g of dimethyl carbonate, heat and stir after sealing the cont...

Embodiment 2

[0029] Lithium difluorooxalate borate was prepared by using lithium fluoride, diboron trioxide and oxalic acid as raw materials.

[0030] Step 1: Put 17.5 g of diboron trioxide and 26 g of lithium fluoride into a ball mill jar, mix and ball mill for 12 hours at 5° C., and the speed of the planetary ball mill is 380 rpm.

[0031] Step 2: Put the ball-milled raw materials above in a muffle furnace, raise the temperature to 400° C. under the protection of nitrogen, and keep the temperature constant for 20 hours to make them react completely.

[0032] Step 3. Transfer the above-mentioned processed raw materials to an appropriate amount of water, stir while heating, and then add 94.8 g of oxalic acid after the mixture is evenly mixed. After the reaction is complete, put the solution into a blast drying oven to remove water to obtain a white product.

[0033] Step 4: Grind the white product finely, then put it into an open reactor, add 1500g of dimethyl carbonate, heat and stir afte...

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Abstract

The invention provides a preparation process of lithium oxalyldifluoroborate (LiODFB) electrolyte salt. The preparation process comprises the following steps: firstly, adding a fluorine-containing salt compound, a lithium-containing compound and a boron-containing compound in a ball-milling pot on the basis that a molar ratio of fluorine to lithium to boron is (2-6): (2-6): (1-3), ball-milling for 2-24 hours at the temperature of 5 DEG C-80 DEG C, and then placing in a muffle furnace, carrying out thermal treatment for 2 hours-24 hours at the temperature of 80 DGE C-850 DEG C; then mixing theraw materials subjected to high-temperature treatment with oxalate in a solvent, and reacting for 1 hour-12 hours at the temperature of 0 DGE C-160 DEG C, wherein the ratio of oxalate to boron is (1-5): (1-3); and finally, purifying with an organic solvent multiple times so as to obtain the required product. The invention has the advantages that the raw materials have low toxicity, low corrosivity, the preparation process is simple and environmentally-friendly and has no strict requirements for equipment on corrosion resistance, high pressure resistance and the like, and is suitable for industrial production in large scale, and investment is less.

Description

technical field [0001] The invention relates to the technical field of manufacturing electrolyte salts of lithium ion batteries, in particular to a preparation method of lithium difluorooxalate borate (LiODFB) electrolyte salts. Background technique [0002] At present, the commercially used lithium salt is lithium hexafluorophosphate (LiPF 6 ), LiPF 6 It is easy to hydrolyze and has poor thermal stability. When it contacts with moisture in the air or residual water in the solvent, it will immediately form HF, which will adversely affect the performance of the battery. Usually LiPF 6 An effective solid electrolyte interphase (SEI) film can be formed on the negative electrode only when it is combined with ethylene carbonate (EC) to form an electrolyte, but the high melting point of EC (37°C) limits the low-temperature performance of the battery. [0003] Now, a lot of research is devoted to the synthesis and application of new lithium salts, hoping to find new substances t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02H01M10/0568
CPCY02E60/12Y02E60/10
Inventor 汤庆华张宝文张禄荪周寅俊
Owner CHANGZHOU GUOYA NEW ENERGY TECH
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