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Phosphazene flame retardant, preparation method thereof and lithium-ion battery electrolyte

A phosphazene flame retardant, lithium ion battery technology, applied in secondary batteries, chemical instruments and methods, secondary battery repair/maintenance, etc., can solve battery capacity loss, flame retardant viscosity, system compatibility problems such as poor performance, to achieve the effect of enhancing stability, improving flame retardant performance, and improving electrical conductivity

Inactive Publication Date: 2013-02-06
湖南有色郴州氟化学有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The Chinese patent literature with the application number 200710028419.8 reports the application of alkyl phosphates in the electrolyte of lithium batteries. The electrochemical compatibility is poor, so when it is used as an additive, it will have a large negative impact on the performance of the battery
Chinese patent CN101694885A discloses an electrolyte of an ethylene bisphthalimide derivative flame retardant. The electrolyte has good flame retardancy, but the cycle performance of the battery is not good
Chinese patent CN101938008A reports the preparation of a 1-alkynyl phosphate flame retardant and the electrolyte containing the flame retardant. The electrolyte has good flame retardant performance, but the battery capacity loss is serious
The Chinese patent literature with the publication number CN101057355A reports that phosphazene compounds are used as lithium battery electrolyte flame retardants. Poor, so when used as a flame retardant, the conductivity of the electrolyte is low, which affects the electrochemical performance of lithium-ion batteries

Method used

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  • Phosphazene flame retardant, preparation method thereof and lithium-ion battery electrolyte
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  • Phosphazene flame retardant, preparation method thereof and lithium-ion battery electrolyte

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preparation example Construction

[0042] Correspondingly, the present invention also provides a preparation method of a phosphazene flame retardant, comprising the following steps:

[0043] Reaction of fluorocarbon alcohol having the structure of formula (IV) with hexachlorocyclotriphosphazene to obtain an intermediate product;

[0044] Rf-OH (IV);

[0045] Wherein, Rf is a fluorine-substituted alkyl group or a fluorine-substituted polyether;

[0046] The intermediate product and HF are fluorinated to obtain a phosphazene flame retardant, and the phosphazene flame retardant has a structure of (I), formula (II) or formula (III):

[0047] Formula (I); Formula (II);

[0048] Formula (III);

[0049] Wherein, Rf is a fluorine-substituted alkyl group or a fluorine-substituted polyether.

[0050] The fluorocarbon alcohol has the structure of formula (IV), wherein Rf is a fluorine-substituted alkyl or a fluorine-substituted polyether, preferably formula (IV-1), formula (IV-2) or formula (IV-3) Compounds sho...

Embodiment 1

[0089] Dissolve 26.4g (0.2mol) of tetrafluoropropanol in 52.8mL of tetrahydrofuran, add 5.04g (0.21mol) of NaH and react under reflux for 5h to obtain sodium tetrafluoropropoxide solution. in N 2 Slowly drop the above sodium tetrafluoropropoxide solution into 69.6g (0.2mol) of hexachlorocyclotriphosphazene in 69.6mL of tetrahydrofuran solution under the protection of the protection of 12h, reflux for 12h, filter, wash with tetrahydrofuran, and the filtrate is washed with anhydrous magnesium sulfate After drying, tetrahydrofuran was removed by atmospheric distillation, and finally 78.2 g of products containing tetrafluoropropyl ether-pentachlorocyclotriphosphazene were obtained by distillation under reduced pressure, with a yield of 88.3%. Among them, tetrafluoropropyl ether-pentachlorocyclotriphosphazene The purity is 95%.

[0090] Add 44.3g (0.1mol) of tetrafluoropropyl ether-pentachlorocyclotriphosphazene and 300g (1.5mol) of anhydrous HF prepared above into a 500mL Monel s...

Embodiment 2

[0095] Get octafluoropentanol 6.4g (0.2mol) and dissolve in 92.8mL tetrahydrofuran, add 5.04g (0.21mol) NaH, the reaction process is the same as in Example 1, obtain the octafluoropentyl-pentachlorocyclotriphosphazene 96.2 g of the product, the yield is 88.6%, and the purity of octafluoropentyl-pentachlorocyclotriphosphazene is 95%.

[0096] 54.3g (0.1mol) of the above-prepared octafluoropentyl-pentachlorocyclotriphosphazene and 300g (1.5mol) of anhydrous HF, the reaction process was the same as in Example 1, and 42.0g of the product was obtained, with a yield of 91.2%. .

[0097] Use NMR to analyze and identify the product, the results are as follows: 1HNMR (400MHz, CDCl3), δ: 3.91(m, 2H, -CH 2 -);δ:5.70(m,1H,-CF 2 H-). 19F NMR (400MHz, CDCl3), δ: -71 (4F); δ: -60 (1F); δ: -138 (2F); δ: -126 (4F); δ: -123 (2F).

[0098] The results showed that the obtained product was octafluoropentyl-pentafluorocyclotriphosphazene with the structure (I-b), and its purity was 99%.

[009...

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Abstract

The invention provides a phosphazene flame retardant, a preparation method thereof and a lithium-ion battery electrolyte. The phosphazene flame retardant is of a structure shown in a formula (I) or a formula (II) or a formula (III), and Rf is fluoro-substitution alkyl or fluoro-substitution polyether. The phosphazene flame retardant comprises N and P and accordingly is good in flame retardant property; the phosphazene flame retardant also comprises a plurality of fluorine atoms, the fluorine atoms and fluoro-substitution alkyl or fluoro-substitution polyether radicals act together, and the flame retardant property of the phosphazene flame retardant is further improved; and the fluoro-substitution alkyl or fluoro-substitution polyether radicals are high in electronegativity, accordingly, the stability and the heat resistance of trimerization phosphazene can be improved, and the electrochemical performance of a battery cannot be degraded when the phosphazene flame retardant is used as an electrolyte flame retardant. The flame retardant can be used for the lithium-ion battery electrolyte, the fluoro-substitution radicals are favorable for increasing flash points of the electrolyte and reducing the viscosity of the electrolyte, and the conductivity of the electrolyte is improved. The formula (I), the formula (II) and the formula (III) are indicated below.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, and more specifically, relates to a phosphazene flame retardant for lithium ion electrolytes, a preparation method thereof and a lithium ion battery electrolyte using the flame retardant. Background technique [0002] Lithium-ion batteries have the characteristics of high energy density, low self-discharge rate, wide operating temperature range, long cycle life, environmental protection, no memory effect, and high current charge and discharge, etc., and are widely used in mobile phones, notebook computers, video cameras, digital cameras At the same time, with the development of science and technology and the enhancement of people's awareness of environmental protection, lithium-ion batteries also show broad application prospects in the fields of new energy vehicles, aerospace, and national defense equipment. [0003] However, when lithium-ion batteries are abused such as overcharge,...

Claims

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Application Information

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IPC IPC(8): H01M10/0567H01M10/42C08G65/335C07F9/6593
CPCY02E60/12Y02E60/10
Inventor 周济苍王刚张新敖明喻京鼎
Owner 湖南有色郴州氟化学有限公司
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