Preparation method of monofluorophosphate

A technology of monofluorophosphate and fluoroalkenyl, which is applied in the field of preparation of high-purity monofluorophosphate, can solve the problems of unfavorable lithium-ion batteries, low purity of additives, and reduced battery capacity and cycle performance, so as to avoid The effect of reducing product yield and improving product yield and purity

Pending Publication Date: 2022-07-01
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0015] As we all know, as a lithium-ion battery electrolyte additive, the purity of the additive is low, and the acidity, heteroion and other indi...

Method used

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  • Preparation method of monofluorophosphate
  • Preparation method of monofluorophosphate
  • Preparation method of monofluorophosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Add 63.9g (1.1mol) potassium fluoride and 172.5g (1mol) diethyl chlorophosphate to the 500mL there-necked flask at room temperature, under nitrogen protection, heat up to 50°C, stir and react for 4 hours, GC detects the raw material chlorination The content of diethyl phosphate is less than 0.2%, and the content of monofluorodiethyl phosphate in the product is 94.2%.

[0046] KCl and excess potassium fluoride were removed by filtration, the filter cake was washed with 30 g of dichloromethane, the filtrate was combined, 3.1 g of calcium oxide was added to the filtrate, stirred for 60 minutes, and the dichloromethane was recovered by atmospheric distillation, and the distillation was stopped after recovery. The rectification device was changed, and 142.5 g of fractions at 87°C were collected under vacuum of 150 hPa.

[0047] After calculation, the product yield was 91.3%, the GC product purity was 99.8%, and no impurities with a content greater than 0.1% were found.

Embodiment 2

[0049]Add 63.9g (1.1mol) potassium fluoride and 172.5g (1mol) diethyl chlorophosphate to the 500mL there-necked flask at room temperature, under nitrogen protection, heat up to 50 DEG C, stir reaction for 4 hours, GC detects raw material chlorination The content of diethyl phosphate is less than 0.2%, and the content of monofluorodiethyl phosphate in the product is 93.8%.

[0050] KCl and excess potassium fluoride were removed by filtration, the filter cake was washed with 30 g of dichloromethane, the filtrate was combined, 4.6 g of sodium carbonate was added to the filtrate, stirred for 60 minutes, and the dichloromethane was recovered by atmospheric distillation, and the distillation was stopped after recovery. The rectification device was changed, and 140.1 g of fractions at 87°C were collected under vacuum of 150 hPa.

[0051] After calculation, the product yield was 89.3%, the GC product purity was 99.5%, and no impurities with a content greater than 0.1% were found.

Embodiment 3

[0053] Add 63.9g (1.1mol) potassium fluoride and 144.5 (1mol) dimethyl chlorophosphate to the 500mL there-necked flask at room temperature, under nitrogen protection, heat up to 50 ℃, stirring reaction 4 hours, GC detects raw material chlorophosphoric acid The content of dimethyl ester is less than 0.2%, and the content of dimethyl monofluorophosphate in the product is 94.6%.

[0054] The potassium chloride and excess potassium fluoride were removed by filtration, the filter cake was washed with 30 g of dichloromethane, the filtrate was combined, 3.1 g of calcium oxide was added, stirred for 60 minutes, the dichloromethane was recovered by atmospheric distillation, the distillation was stopped after recovery, and the rectification was changed. device, and collect 116.1 g of 79°C fraction under vacuum of 150 hPa.

[0055] After calculation, the product yield was 90.7%, the GC product purity was 99.6%, and no impurities with a content greater than 0.1% were found.

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Abstract

The invention discloses a preparation method of monofluorophosphate, which comprises the following steps: a stabilizer is added into an obtained monofluorophosphate reaction solution, the stabilizer is selected from at least one of metal oxide, anhydrous carbonate and anhydrous bicarbonate, and the structure of the monofluorophosphate is as shown in the following formula (I), in the formula (I), R is selected from C1-C6 alkyl groups, C1-C6 fluoroalkyl groups, C2-C6 alkenyl groups and C2-C6 fluoroalkenyl groups. The prepared monofluorophosphate product is high in yield, high in purity, low in acidity and low in impurity content.

Description

technical field [0001] The invention relates to the synthesis of lithium ion battery electrolyte additives, in particular to a preparation method of high-purity monofluorophosphate. Background technique [0002] Fluorophosphate compounds are often used as additives in lithium-ion battery electrolytes, which have the effect of inhibiting gas production and help to improve the performance of normal temperature cycling, high temperature storage and high temperature cycling. Monofluorophosphate is a kind of fluorophosphate compound, and its preparation route mainly includes the following two: [0003] 1) Monochlorophosphate route [0004] Taking monochlorophosphoric acid ester and fluorinated reagent as raw materials, react in the presence of solvent, and the reaction formula is as follows: [0005] [0006] Patent JP2017119690A discloses a method for obtaining diethyl fluorophosphate by reacting diethyl chlorophosphate and potassium fluoride in an acetonitrile solvent. In ...

Claims

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Application Information

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IPC IPC(8): C07F9/14
CPCC07F9/14C07F9/025
Inventor 姚汉清韦伟李晶吴海峰蒋云菊尚雁
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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