Electrochemical fluorination preparation method of hydrogen fluoride ether

Abstract

The invention relates to a preparation method of hdrogen fluoride ether, in particular to an electrochemical fluorination preparation method of hydrogen fluoride ether. A chloroether compound, a fluorination reagent and an aprotic solvent are added into a fluorination electrolytic cell for fluorination to generate a chlorine-free hydrogen fluoride ether product, and the fluorination reagent is Et3N-3HF; the aprotic solvent is dimethyl sulfoxide; the concentration of the Et3N-3HF in the dimethyl sulfoxide ranges from 10 to 15 mol / L; the electrode voltage of the fluorination electrolytic cell iscontrolled at 3.5 V. By the use of the Et3N-3HF, the selective fluorination performance is extremely high, and the product contains fewer impurities, is higher in purity, and is higher in yield underhigh selectivity; by the adding of the aprotic solvent, in the initial stage of electrolysis, relatively good influence is generated on the conductivity of the solution. According to the electrochemical fluorination preparation method of the hydrogen fluoride ether, by chloroether compound serving as a main raw material, various hdrogen fluoride ether compounds such as perfluoroethyl methyl ethercan be prepared; furthermore, the reaction replacement selectivity is improved; after post-treatment, the content of target products in the prepared product is 99.9 percent.

Description

technical field [0001] The invention relates to a method for preparing hydrofluoroether, in particular to a method for preparing hydrofluoroether by electrochemical fluorination. Background technique [0002] Fluorine-containing chemicals show many advantages, such as partially fluorinated or fully fluorinated organic compounds have unique properties such as insulation, hydrophobicity and oil repellency, and high temperature resistance, so fluorine-containing compounds are very commercially valuable chemicals. It has important and special uses in the fields of medicine, new materials, and pesticides. Hydrofluoroethers are a class of partially fluorinated fluorine-containing compounds that can be used as cleaning agents, foaming agents, refrigerants, etc. [0003] There are many methods for preparing hydrofluoroethers, including alkylation of carboxyl compounds, addition of fluorine-containing olefins and alcohols, etc., all of which have disadvantages in terms of raw materi...

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Problems solved by technology

[0005] People then searched for a milder fluorination reagent as an electrolyte for another electrochemical fluorination method. This method was proposed by Schmidt in the 1950s. After continuous exploration by people in the later period, the exchange reaction of fluorine and halogen atoms was realized. , such as 2006 Sanit-Jalmes et al reported using triethylamine tri(hydrogen fluoride) (Et 3 N-3HF) can carry out selective fluorine-chlorine exchange reaction to produce cyclic hydrofluorosulfides. The target products are all aromatic compounds. The boiling point is generally higher than 100 °C, but the yield is very low, generally not more than 10 %

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