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A kind of preparation method of phosphinate, phosphinate and non-aqueous electrolyte

A technology of phosphinate and intermediates, which is applied in the field of preparation of phosphinate, and can solve the problem of few synthetic methods

Active Publication Date: 2020-07-28
微宏先进材料公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The application value of phosphinate has attracted increasing attention, but there are few studies on its synthesis method

Method used

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  • A kind of preparation method of phosphinate, phosphinate and non-aqueous electrolyte
  • A kind of preparation method of phosphinate, phosphinate and non-aqueous electrolyte
  • A kind of preparation method of phosphinate, phosphinate and non-aqueous electrolyte

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] The first step of reaction: add 170.0g of phosphorous trichloride and 1.5L solvent tetrahydrofuran to the reaction vessel, and stir evenly at room temperature, then add the tetrahydrofuran solution containing 191.0g of n-butylmagnesium bromide and continue stirring for 18h to obtain a reaction solution . The reaction solution was poured into 500 mL of 10 wt % sulfuric acid solution, extracted with ether and separated to obtain an organic layer, dried with anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain a solid mixture. The solid mixture was recrystallized from toluene and ethanol to give a white solid, which was dried in vacuo to give 74.0 g of product

[0069] The second step reaction: transfer 70.0g of the above product to a single-necked round-bottomed flask, add 85.9g of antimony trifluoride and start stirring, and connect the single-necked round-bottomed flask to a vacuum distillation device, and heat it to 165°C un...

Embodiment 2

[0075] The first step and the second step reaction are the same as in Example 1, and the difference is that the third step reaction is that the 36g colorless liquid product Transfer to a two-necked round-bottomed flask, keep the reaction vessel connected to the air, so as to utilize the moisture in the air, slowly stir at 27°C for 0.5 hours, then slowly stir and add 15.8g of n-butanol within 0.5 hours, at room temperature at 27°C React 1h to the end of the reaction. Obtain 33.3g (yield is 80%) product by distillation under reduced pressure

[0076] Non-aqueous electrolyte preparation: prepare non-aqueous mixed solvents of ethylene carbonate (EC), ethyl methyl carbonate (EMC) and dimethyl carbonate (DMC), the volume ratio of EC:EMC:DMC is 30:50:20, and then add to it (the content is 5.0 wt% of the mass of the non-aqueous electrolytic solution) and the film-forming additive vinylene carbonate (VC, the content of which is 2.0 wt% of the mass of the non-aqueous electrolytic ...

Embodiment 3

[0080] The first step reaction: add 170.0 g of phosphorous trichloride and 1.5 L of solvent tetrahydrofuran into the reaction vessel, and stir evenly at room temperature (25° C.). Then add 399.1 g of ethylmagnesium bromide in tetrahydrofuran (399.1 g refers to the mass of ethylmagnesium bromide) and continue to stir at 25°C until the reaction lasts for 48 hours to obtain a reaction solution. The reaction solution was poured into 500 mL of 10 wt% sulfuric acid solution, extracted with ether and separated to obtain an organic layer, which was dried with anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain a solid mixture. The solid mixture was recrystallized from toluene and ethanol to give a white solid, which was dried in vacuo to give 69.0 g of product

[0081] The second reaction step: transfer 69.0 g of the above product to a single-necked round bottom flask, add 108.0 g of antimony trifluoride and start stirring. And the single...

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Abstract

The invention provides a preparation method of phosphinic acid ester, phosphinic acid ester and its non-aqueous electrolyte. The preparation method of said phosphinate ester includes the following steps: (1) passing Grignard reagent R 1 MgX and trihalothionophosphorus 3 P=S reacts in the solvent to obtain the first intermediate; (2) through the halogenating agent M’X a React with the first intermediate to obtain a second intermediate; (3) through R 2 OH, water react with the second intermediate to obtain phosphinate; wherein, R 1 ,R 2 Respectively selected from hydrocarbon groups, or organic groups containing at least one element among boron, silicon, nitrogen, phosphorus, oxygen, sulfur, fluorine, chlorine, bromine and iodine; X represents halogen; M' represents a metal element; a represents a metal element The valence of M'. The electrolyte prepared using the phosphinate ester of the present invention can improve the high-temperature cycle stability of secondary batteries; it also has non-combustible, flame-retardant or self-extinguishing properties, and can improve the safety performance of secondary batteries.

Description

technical field [0001] The invention relates to a preparation method of phosphinate, phosphinate and nonaqueous electrolytic solution. Background technique [0002] In the field of lithium-ion secondary battery applications, safety performance is always a "stumbling block", such as fire incidents in the field of electric vehicles. The main cause of electric vehicle fires is the lithium-ion secondary battery it uses, and one of the reasons for the battery fire is the flammable non-aqueous electrolyte it uses. In addition, the life of lithium-ion secondary batteries, especially the capacity retention rate under high temperature conditions, cannot meet the needs of current practical applications. [0003] So far, there have been many literature reports that phosphinates are used as film-forming additives, flame-retardant additives or non-flammable solvents in electrolytes to improve the high-temperature characteristics and safety performance of lithium / sodium-ion secondary bat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/32C07F9/6568H01M10/0567
CPCC07F9/3258C07F9/3264C07F9/65681H01M10/0567Y02E60/10
Inventor 臧旭峰钮博翔邢玉金周晓蒙李中凯郑卓群
Owner 微宏先进材料公司
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