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Flame-retardant lithium ion battery electrolyte and method for preparing same

A lithium-ion battery, flame-retardant technology, applied in the direction of secondary batteries, circuits, electrical components, etc., can solve the problems of poor compatibility with the negative electrode, low cost of synthesis, good wettability, good The effect of flame retardancy and even non-combustibility

Active Publication Date: 2012-07-18
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of phosphate (sub) ester electrolyte has the characteristics of low price, non-combustibility, low toxicity, high electrical conductivity, and good electrochemical stability. However, this type of organic phosphorus compound has poor compatibility with graphite carbon negative electrodes and needs Further improve
Chinese patent CN10193808A reports a flame retardant containing alkyne-containing phosphoric acid ester, which has good electrochemical performance, but its compatibility with the negative electrode still needs to be improved

Method used

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  • Flame-retardant lithium ion battery electrolyte and method for preparing same
  • Flame-retardant lithium ion battery electrolyte and method for preparing same
  • Flame-retardant lithium ion battery electrolyte and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The synthetic method of N, N-diallyl-diethoxyphosphoramide (DEDAPA):

[0048] In a 250mL three-necked flask, 8.63g (50mmol) of diethoxyphosphoryl chloride and 8.5mL (60mmol) of triethylamine were dissolved in 100mL of anhydrous acetonitrile, and 5.8g (60mmol) of diallyl The amine was reacted at room temperature for 5 h, extracted, and the organic phase was collected, dried, and distilled under reduced pressure to obtain 11.2 g of the product, with a yield of 96%. Using ESI-MS, 1 HNMR, 13 C NMR and 31 The product was characterized by P NMR, and the result confirmed that it was the target product. Data are as follows:

[0049] 1 H NMR (CDCl 3 , 400MHz): δ5.81-5.68(m, 2H), 5.21-5.12(m, 4H), 4.12-3.96(m, 4H), 2.55(d, J=9.6Hz, 4H), 1.06(t, J = 7Hz, 6H); 13 C NMR (CDCl 3 , 100MHz): δ134.5, 117.7, 62.1 (d, J C-P =6.2Hz), 47.6(d, J C-P =4.2Hz), 16.1(d, J C-P =7.3Hz); 31 P NMR (CDCl 3 , 162MHz): δ13.49.ESI-MS: m / z=234[M+H] + ;256[M+Na] + .

Embodiment 2

[0051] N-methyl-N-allyldiethoxyphosphoramide (DEAMPA) synthetic method 1:

[0052] In a 250mL three-necked flask, 8.63g (50mmol) of diethoxyphosphoryl chloride and 8.5mL (60mmol) of triethylamine were dissolved in 100mL of anhydrous acetonitrile, and 4.3g (60mmol) of methallyl was added dropwise under ice-cooling conditions. base amine, reacted at room temperature for 5 h, extracted, collected the organic phase, dried, and distilled under reduced pressure to obtain 9.8 g of the product, with a yield of 95%.

[0053] N-methyl-N-allyldiethoxyphosphoramide (DEAMPA) synthetic method two:

[0054] In a 250 mL three-necked flask, dissolve 8.63 g (50 mmol) of diethyl hydrogen phosphite, 8.5 mL (60 mmol) of triethylamine and 4.3 g (60 mmol) of methallylamine in 80 mL of acetonitrile, and slowly Slowly add 23g of carbon tetrachloride dropwise, react at room temperature for 5h, extract, collect the organic phase, dry, and distill under reduced pressure to obtain 9.3g of the product, wi...

Embodiment 3

[0059] The alkenylphosphoramide contained in this example is a phosphorus-containing organic compound with the following structural formula:

[0060]

[0061] That is, the R in the general formula 1 , R 2 Both are ethyl, R 3 , R 4 Allyl, the above compound named N, N-diallyl-diethoxyphosphoramide, referred to as DEDAPA.

[0062] lithium salt LiPF 6 Soluble in solvent (EC:DMC=1:1) and additive DEDAPA, in which LiPF 6 Accounting for 10%, the content of DEDAPA is 2.5%, 5%, 10%, 20% respectively, the rest is solvent, and the electrolytes are respectively named 2.5% DEDAPA, 5% DEDAPA, 10% DEDAPA, 20% DEDAPA; and DEDAPA accounts for 10% , LiPF 6 5%, 10%, 20%, and the rest are solvent electrolytes, named DEDAPA-5% LiPF respectively 6 , DEDAPA-10%LiPF 6 , DEDAPA-20%LiPF 6 .

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Abstract

The invention discloses a flame-retardant lithium ion battery electrolyte and a method for preparing the same and relates to a battery electrolyte. The electrolyte has the characteristic of flame retardance and complete non-combustion and is well compatible with an electrode material, and the wettability of a diaphragm can be improved. The flame-retardant lithium ion battery electrolyte comprises 5 to 20 percent of lithium salt, 60 to 90 percent of solvent and 1 to 20 percent of alkenyl phosphamide. The method comprises the following steps of: reacting dialkoxyl phosphoryl chloride and alkenyl-containing secondary amine, or hydro-diphosphite, the alkenyl-containing secondary amine, carbon tetrachloride and alkali, which are taken as raw materials, in an organic solvent to obtain an alkenyl phosphamide compound; and preparing the alkenyl phosphamide compound, the lithium salt and the solvent to obtain the flame-retardant lithium ion battery electrolyte.

Description

technical field [0001] The invention relates to a battery electrolyte, in particular to a flame-retardant lithium-ion battery electrolyte containing alkenyl phosphoramide additives and a preparation method thereof. Background technique [0002] Since the 1990s, after Sony Corporation of Japan began to realize the commercial production of lithium-ion batteries, lithium-ion batteries have been used in many industries due to their high specific energy, high energy density, small self-discharge, long cycle life, and less environmental pollution. Portable electronic products are widely used in the market, and are currently being developed and applied to the power supply of hybrid electric vehicles and the field of smart grids. However, the safety issue of lithium-ion batteries is still one of the important factors restricting its large-scale development and application. One of the origins of the safety problems of lithium-ion batteries is that they use flammable organic electrol...

Claims

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Application Information

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IPC IPC(8): H01M10/0567
CPCY02E60/12Y02E60/10
Inventor 杨勇赵玉芬曹霞李秀斌高玉兴唐果
Owner XIAMEN UNIV
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