A kind of preparation method of perfluorocyclohexyl fluoride

Abstract

The invention discloses a preparation method of perfluorocyclohexylformyl fluoride. (a) by volume, 5-6 parts of electrolyte, 15-16 parts of anhydrous hydrofluoric acid and 2-3 parts of solubilizer are put into the Reaction kettle, under the conditions of temperature 10-25°C and pressure 0.05-0.15MPa, react for 1-5 hours to obtain the electrolytic configuration solution, which is ready for use; (b) continuously add the electrolytic configuration solution obtained in step (a) to the circulation tank , and then fed into the electrolytic cell through a circulating pump, and the electrolytic fluorination reaction is carried out at a temperature of 15-35 °C under normal pressure. The gas phase product obtained by electrolysis enters the product condenser through the pipeline, and the liquid phase condensed by the product condenser enters the product separator for stratification. The upper inorganic phase is hydrogen fluoride, which is sent to the circulation tank to participate in the electrolytic fluorination reaction again. The lower inorganic phase After filtration and rectification, the product of perfluorocyclohexylformyl fluoride is obtained. The invention has the advantages of simple process, long operation period, stable product quality, energy saving and environmental protection.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing compounds, in particular to a preparation method of perfluorocyclohexylcarbonyl fluoride. Background technique [0002] Perfluorocyclohexylcarbonyl fluoride is the main raw material for the synthesis of high-grade fluoropolymer initiators, and can also be used to synthesize other high-efficiency new initiators for plastics, new fluorine-containing liquid crystal materials, and various fluorine-containing surface active materials. agent etc. [0003] Currently, the most commonly used method for the preparation of perfluorocyclohexylcarbonyl fluoride is electrolytic fluorination in anhydrous hydrogen fluoride medium with nickel anode, which can convert non-fluorinated or partially fluorinated organic compounds into perfluorinated analogues, And it can retain the functional group or structure of the original compound with the heteroatom group in the molecule. The essence of the electro...

AI Technical Summary

Problems solved by technology

However, mercaptan has a pungent and unpleasant smell, and the production environment is harsh

In addition, it should be pointed out that the above-mentioned sulfur-containing compounds are prone to electrolytic fluorination, and there are a large number of perfluorinated hydrolytically unstable hexavalent sulfur compounds in the semi-finished products, resulting in poor product quality

In addition, the industrial application of perfluorinated hydrolytically unstable hexavalent sulfur compounds is limited, and the target product can only be treated as waste after separation, which increases the discharge of three wastes