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Preparation method of pentafluoroethoxycyclotriphosphazene

A technology for pentafluoroethoxy cyclotriphosphazene and hexafluoro cyclotriphosphazene, which is applied in the field of preparation of pentafluoroethoxy cyclotriphosphazene, can solve the problem of many by-products such as amino substituents and diethyl by-product There are many problems such as oxygen substitution and lower yield, so as to achieve the effects of low reaction temperature, high conversion rate and few by-products

Active Publication Date: 2019-03-05
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The defect of this method is: hexafluorocyclotriphosphazene reacts with ethanolate, and the by-product diethoxy substituents are more, which greatly reduces the yield
The defect of this method is: there are many by-products such as amino substituents, which also greatly reduces the yield

Method used

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  • Preparation method of pentafluoroethoxycyclotriphosphazene
  • Preparation method of pentafluoroethoxycyclotriphosphazene
  • Preparation method of pentafluoroethoxycyclotriphosphazene

Examples

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preparation example Construction

[0022] The preparation method of pentafluoroethoxycyclotriphosphazene is described in detail below.

[0023] Pentafluoroethoxycyclotriphosphazene, its structural formula is as follows:

[0024]

[0025] The preparation method of pentafluoroethoxycyclotriphosphazene comprises the following steps: 1. Add reactants hexafluorocyclotriphosphazene and ethanol in an organic solvent, add a catalyst and an acid-binding agent, and obtain a reaction solution after the reaction is completed; 2. Filtrate the reaction solution to obtain a filtrate, and rectify the filtrate to obtain the target product pentafluoroethoxycyclotriphosphazene.

[0026] Described organic solvent is n-hexane, cyclohexane, toluene, xylene, chlorobenzene, acetonitrile, acetone, tetrahydrofuran, dioxane, petroleum ether, ethyl acetate, dichloroethane, dimethyl carbonate, carbonic acid Any of the diethyl esters. The organic solvent is preferably any one of n-hexane, acetonitrile, dimethyl carbonate, and dichloroe...

Embodiment 1

[0033] Example 1. The preparation method of pentafluoroethoxycyclotriphosphazene comprises the following steps: 1. In a 2000ml three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 600g of organic solvent n-hexane, and reactant hexafluorocyclotriphosphazene 200g of triphosphazene and 37g of ethanol were added, and 6g of main catalyst KI, 4g of cocatalyst tetrabutylammonium bromide, and 85g of acid-binding agent sodium carbonate were added. The reaction temperature was controlled at 25°C, and the reaction was carried out for 4 hours. After the reaction, a reaction liquid was obtained. Sampling was carried out to analyze the purity. The content of pentafluoroethoxycyclotriphosphazene was 25.8%, and the conversion rate of hexafluorocyclotriphosphazene was 95.88%. 2. The reaction liquid is filtered to obtain a filtrate, and the filtrate is rectified to obtain the target product high-purity (99.9%) pentafluoroethoxycyclotriphosphazene.

Embodiment 2

[0034] Example 2. The preparation method of pentafluoroethoxycyclotriphosphazene comprises the following steps: 1. In a 2000ml three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 600 g of organic solvent acetonitrile, and reactant hexafluorocyclotriphosphazene Phosphazene 200g and ethanol 37g, and add main catalyst NaI 12g, cocatalyst tetramethylammonium chloride 6g, acid-binding agent potassium carbonate 111g, reaction temperature is controlled at 30 ℃, reacts for 4 hours, obtains reaction liquid after reaction finishes. Sampling was carried out to analyze the purity. The content of pentafluoroethoxycyclotriphosphazene was 26.1%, and the conversion rate of hexafluorocyclotriphosphazene was 97.03%. 2. The reaction liquid is filtered to obtain a filtrate, and the filtrate is rectified to obtain the target product high-purity (99.9%) pentafluoroethoxycyclotriphosphazene.

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Abstract

The invention discloses a preparation method of pentafluoroethoxycyclotriphosphazene. The preparation method comprises the following steps: (1) adding reactants including hexafluorocyclotriphosphazeneand ethanol to an organic solvent, and adding a catalyst and an acid binding agent so as to obtain a reaction liquid after completion of a reaction; and (2) filtering the reaction liquid so as to obtain a filtrate, and rectifying the filtrate so as to obtain the target product pentafluoroethoxycyclotriphosphazene, wherein the organic solvent is an arbitrary one of n-hexane, cyclohexane, toluene,xylene, chlorobenzene, acetonitrile, acetone, tetrahydrofuran, dioxane, petroleum ether, ethyl acetate, dichloroethane, dimethyl carbonate and diethyl carbonate, and the catalyst comprises a main catalyst and a cocatalyst; and the main catalyst is alkali metal iodide, the cocatalyst is a phase transfer catalyst, and the acid binding agent is an arbitrary one of sodium carbonate, potassium carbonate, ammonia and triethylamine. The preparation method of pentafluoroethoxycyclotriphosphazene has a low reaction temperature, few by-products and a high conversion rate.

Description

technical field [0001] The invention relates to a preparation method of pentafluoroethoxycyclotriphosphazene. Background technique [0002] Pentafluoroethoxycyclotriphosphazene, its structural formula is as follows: [0003] [0004] Pentafluoroethoxycyclotriphosphazene is one of the flame retardants in lithium battery electrolyte and has good flame retardant effect. [0005] The invention application with application number 2014106844282 discloses a synthesis method of pentafluoroethoxycyclotriphosphazene: first fluorinate hexachlorocyclotriphosphazene with a fluorinating agent to form hexafluorocyclotriphosphazene, and then fluorinate hexafluorocyclotriphosphazene Cyclotriphosphazene reacts with ethanolate to form pentafluoroethoxycyclotriphosphazene. The defect of this method is that: hexafluorocyclotriphosphazene reacts with ethanolate, and the by-product diethoxy substitutes more, which greatly reduces the yield. [0006] A commonly used method for preparing penta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593
CPCC07F9/65815
Inventor 陈晓华岳立时二波刘栋成常楠周铭柯
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD