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Five-membered ring phosphate compound, and preparation method and application thereof

A five-membered cyclic phosphate and compound technology, applied in the field of flame retardant, can solve the problems of poor flame retardant effect, affecting the cycle performance and safety performance of secondary batteries, and achieve improved battery safety, enhanced flame retardant ability, and improved Effect of high voltage withstand capability

Pending Publication Date: 2020-06-02
EVERGRANDE NEW ENERGY TECH SHENZHEN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a five-membered cyclic phosphate compound, which aims to solve the problem of poor flame retardant effect in existing non-aqueous electrolyte phosphorus-containing flame retardants, which affects the cycle performance and safety performance of secondary batteries, etc. performance problem

Method used

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  • Five-membered ring phosphate compound, and preparation method and application thereof
  • Five-membered ring phosphate compound, and preparation method and application thereof
  • Five-membered ring phosphate compound, and preparation method and application thereof

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[0048] The embodiment of the present invention also provides a method for preparing a five-membered cyclic phosphate compound, comprising the following steps:

[0049] S10. Dissolving compound A in a non-aqueous solvent, adding phosphorus oxychloride to react, and separating to obtain compound B;

[0050] S20. After mixing the compound B and the compound C, react at a temperature of -40°C to 60°C to separate and obtain a five-membered ring phosphate compound;

[0051] Wherein, the reactant A is selected from: and / or The reactant C is selected from: and / or

[0052] Among them, R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 , R 10 , R 11 , R 12 , R 13 , R 14 , R 15 , R 16 , R 17 and R 18 are independently selected from: hydrogen, alkyl, alkenyl, alkynyl, alkoxy, alkynyloxy, alkenyloxy, silyl, siloxane, haloalkyl, phenyl, biphenyl, naphthyl, Pyridyl, thienyl, halogenated phenyl, halogenated biphenyl, phenol, alkyl-containing phenol, alkenyl-con...

Embodiment 1

[0092] In order to be able to compare the preparation process of the more intuitive comparison products in parallel, the same self-made compound B (that is, the compound B prepared in Example 1) was used in Examples 2 to 33 of the present invention. The specific preparation process includes:

[0093] ①At room temperature, add 62g of ethylene glycol (reactant A) and 400g of anhydrous dichloromethane (non-aqueous solvent) into a three-neck flask with a volume of 1000mL in a fume hood, then cool down to 0°C, and keep stirring for 0.5h. At this time, the solution is colorless and transparent, and the three-necked bottle is connected to an external gas absorption device.

[0094] ② Slowly add 300g of phosphorus oxychloride dissolved in 300g of anhydrous dichloromethane into the there-necked bottle through the dropping funnel, and control the dropping rate to 1 drop / second. With the continuous dropwise addition of the dichloromethane solution of phosphorus oxychloride, the reaction ...

Embodiment 2

[0098] Compound 1 ( Preparation of two (2-oxo-1,3,2-dioxaphospholane) glycol esters):

[0099] Add 400g of dichloromethane (solvent, the same effect as the aforementioned non-aqueous solvent, optional use) and 62g of ethylene glycol (reactant C) into a 1000mL three-necked flask at room temperature, the solution is colorless and transparent, and the three-necked flask is connected Connect an external gas absorption device, then slowly add 300g of compound B prepared in Example 1 into a 1000mL three-necked flask through a dropping funnel, control the dropping rate at 1 drop / second, and the reaction temperature at 0°C. With the dropwise addition of compound B, A large amount of heat is released and a large amount of HCl gas is released. After all the drops are completed, the solution is colorless and transparent (dropping compound B to this point for 1.5h), and then the reaction is slowly raised to room temperature and continued to stir for 12h. The light yellow solid was obtai...

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Abstract

The invention belongs to the technical field of flame retardance, and especially relates to a five-membered ring phosphate compound. The structural general formula of the five-membered ring phosphatecompound is represented by formula 1 shown in the description; and in the formula, R<1>, R<2>, R<3>, R<4>, R<5>, R<6>, R<7>, R<8>, R<9>, R<10>, R<11>, R<12>, R<13>, R<14>, R<15>, R<16>, R<17> and R<18> are independently selected from hydrogen, an alkyl group, an alkenyl group, an alkynyl group, an alkoxy group, an alkynyloxy group, an enyloxy group, a silyl group, a siloxane group, aryl silicon, an arylsilyl group, an arylsiloxy group, a halogenated phenyl group, a halogenated biphenyl group, a phenolic group, an alkyl-containing phenolic group, an alkenyl-containing phenolic group, an alkynyl-containing phenolic group, a nitrile-containing phenolic group, a monohalogenated phenolic group and a polyhalogenated phenolic group. The five-membered ring phosphate compound provided by the invention has excellent flame retardancy, can effectively prevent electrolytes from being oxidized when being applied to the field of batteries, reduces oxygenolysis of the electrolytes on positive electrodes, and remarkably improves the comprehensive properties of high temperature, circulation, storage and the like of the batteries.

Description

technical field [0001] The invention belongs to the field of flame retardant technology, and in particular relates to a five-membered cyclic phosphate compound and a preparation method thereof, a flame retardant containing the five-membered cyclic phosphate compound, containing the five-membered cyclic phosphate compound or An electrolyte solution of a flame retardant, and a secondary battery containing the electrolyte solution. Background technique [0002] Due to its light weight, high specific energy density, high open circuit voltage, long service life, and low self-discharge rate, secondary batteries are widely used in digital products, smart wear, medical care, new energy vehicles, navigation, aerospace and other fields. With the continuous deepening of people's research on secondary batteries, the secondary battery industry has developed rapidly, especially in the emerging power and energy storage fields, secondary batteries are increasingly showing their unique advan...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C09K21/12H01M10/0567H01M10/42H01M10/0525
CPCC07F9/65742C09K21/12H01M10/0567H01M10/4235H01M10/0525H01M2300/0025Y02E60/10
Inventor 时迎华赵文文张勍李浚秀
Owner EVERGRANDE NEW ENERGY TECH SHENZHEN CO LTD
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