PURPOSE: To produce an org. perfluorochemical by treating a fluoride obtained by fluorinating an org. compd. in an electrolytic bath with gaseous fluorine.

CONSTITUTION: An org. compd. having a carbon-hydrogen bond is electrolytically fluorinated to obtain the fluoride, and the fluoride is fluorinated with gaseous fluorine to obtain an org. perfluorochemical and a gaseous mixture contg. hydrogen fluoride and unreacted gaseous fluorine. The gaseous fluorine in the gaseous mixture is removed, and the recovered hydrogen fluoride is used in electrolytic fluorination. Consequently, the consumption of hydrogen fluoride used as the material for the fluorination reaction as a combination of electrolytic fluorination and direct fluorination is reduced.