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A kind of preparation method of flame retardant electrolyte

A technology of electrolyte and flame retardant performance, which is applied in the field of preparation of lithium battery flame retardant electrolyte, which can solve the problems of carbon negative electrode stripping, no flame retardant lithium salt, affecting battery cycle performance, etc.

Active Publication Date: 2022-05-17
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Trimethyl phosphate (TMP) and triethyl phosphate (TEP) are the earliest researched flame retardant additives used in lithium-ion batteries. They have good flame retardant effects, but due to their high phosphorus content, they are easy to cause the carbon negative electrode to peel off. Affect the cycle performance of the battery
At present, there are no reports of flame retardant lithium salts

Method used

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  • A kind of preparation method of flame retardant electrolyte
  • A kind of preparation method of flame retardant electrolyte
  • A kind of preparation method of flame retardant electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] [Example 1]: Partially substituted phosphate ester substituted cyclotriphosphonitrile [Cl x (-CP-) 3 (PO 3 R’ 2 ) 6-x ] preparation

[0044] Start with [Cl 3 (-CP-) 3 (PO 3 Et 2 ) 3 ] preparation as an example

[0045]Respectively, 0.1 mol hexachlorocyclotrile (34.8g) and 0.3 mol triethyl phosphite (49.8g), dissolved to 100mL and 200mL xylene (dried), stirred under the condition of mixing the two solutions mixed in a three-mouth flask with agitator, condensing tube and heating device 1L, stirred, reacted at 80 ~ 100 ° C for 5 to 7h, steamed out of the solvent, cooled, washed with an appropriate amount of petroleum ether 3 to 4 times to remove impurities, filtration, The crude product was recrystallized 3 times with ethanol to obtain a colorless solid, dried at 60 ~ 100 ° C in a vacuum drying box to give a solid powdered product [Cl]. 3 (-CP-) 3 (PO 3 Et 2 ) 3 ]。

[0046] Using the same method, the raw material ratio of different molar ratios can be [Cl x (-CP-) 3 (PO 3 Et ...

Embodiment 2

[0048] [Example 2]: intermediate [(R-Ar-O) x (-CP-) 3 (PO 3 R’ 2 ) 6-x ] compositing

[0049] Start with [ ( (CH 3 ) 2 CH-ph-O) 3 (-CP-) 3 (PO 3 Et 2 ) 3 ] synthesis as an example:

[0050] In a three-mouth flask equipped with electric stirring, condensing tube and nitrogen protection, the product obtained in accordance with Example 1 [Cl 3 (-CP-) 3 (PO 3 Et 2 ) 3 0.1mol (46.95g) is dissolved into tetrahydrofuran, the solution is slowly added dropwise to 0.11mol (17.38g) of the sodium salt of isopropylphenol tetrahydrofuran solution, stirred at 80 ° C for 24h to be completed, cooled, neutralized with glacial acetic acid to neutral, standing in an ice water bath, cooling, crystal precipitation, filtering, the resulting crude product with tetrahydrofuran for recrystallization, to obtain pure white crystals [((CH 3 ) 2 CH-ph-O) 3 (-CP-) 3 (PO 3 Et 2 ) 3 ]。

[0051] The same method is simply chosen to use [Cl x (-CP-) 3 (PO 3 Et 2 ) 6-x ] (x is an integer in 1 to 5) replace isopropyl ph...

Embodiment 3

[0053] [Example 3]: intermediate [(R-Ar-O) x ((-CP-) 3 (PO 3 R’ 2 ) 6-x ] hydrolysis reaction to prepare a novel flame retardant lithium salt [(R-Ar-O) x (-CP-) 3 (PO 3 Li 2 ) 6-x ]

[0054] [Method 1] Hydrolyzed in lithium hydroxide solution

[0055] This method requires an excess of lithium hydroxide, weighing a certain amount of [(R-Ar-O) x (-CP-) 3 (PO 3 R’ 2 ) 6-x Disperse into 2mol / L lithium hydroxide solution, heat, stir, reflux for 24h, distill the ethanol produced by hydrolysis reaction, continue to concentrate, cool, stand overnight, to obtain a crude product, the crude product is recrystallized twice with a mixture of ethanol and water, to obtain colorless crystals [(R-Ar-O) x (-CP-) 3 (PO 3 Li 2 ) 6-x ]。 The mother liquor is exchanged with cation exchange resin to collect and recover lithium ions.

[0056] [Method 2] Hydrolyzed in sodium hydroxide solution. The same method as method one, just replace the lithium hydroxide solution with a sodium hydroxide solution, resu...

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Abstract

A method for preparing a flame-retardant electrolyte. The flame-retardant electrolyte easily soluble in an organic solvent is to use hexachlorocyclotriphosphazene (HCCP) to replace part of the chlorine with an alkyl aromatic hydrocarbon oxygen group, and the remaining chlorine is replaced by a phosphite. Obtain the cyclotriphosphazene lithium phosphate [(R-Ar-O) substituted with part of the aromatic x (‑CP‑) 3 (PO 3 Li 2 ) 6‑x ]((‑CP‑) 3 is a cyclotriphosphazene ring, x is a positive integer from 1 to 5). [(R‑Ar‑O) x (‑CP‑) 3 (PO 3 Li 2 ) 6‑x ] and [(R‑Ar‑O) x (‑CP‑) 3 (PO 3 R' 2 ) 6‑x ] Compounding according to the mass ratio of 10:1-1:1, dissolving in an organic solvent in an amount of 6%-48% to obtain a flame-retardant electrolyte. The electrolyte has good lithium ion conductivity and good flame retardancy, and is used for various lithium batteries.

Description

Technical field [0001] The present invention relates to a kind of preparation of a flame retardant electrolyte for lithium batteries. The lithium salt in the electrolyte has good solubility in organic solvents, high conductivity, flame retardant function, and plays an important role in improving the safety performance of lithium-ion batteries. Can be used for lithium-ion batteries, lithium-oxygen batteries, lithium-sulfur batteries. Background [0002] Electrolyte is an important part of electrochemical energy devices such as lithium-ion batteries, lithium-oxygen batteries, and lithium-sulfur batteries, and plays an important role in transmitting ions to ensure the electron transmission of the electrochemical devices' yin and yang polar reactions. Especially in the context of large-scale application of lithium-ion batteries, the safety of large-capacity lithium-ion batteries has become an important research topic. [0003] In lithium-ion batteries, the electrolyte, as an importa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/052H01M10/0567H01M10/0569H01M10/42C07F9/659
CPCH01M10/052H01M10/0567H01M10/0569H01M10/4235C07F9/65815H01M2300/0028Y02E60/10
Inventor 李忠芳孙鹏崔伟慧王传刚郭辉王燕
Owner SHANDONG UNIV OF TECH