To provide a process for safely producing a perfluoroacyl peroxide with good productivity.By supplying a perfluoroacyl halide-containing organic solvent solution, an aqueous solution of hydrogen peroxide or a metal peroxide, and an aqueous basic alkali metal compound solution to a tubular reactor to allow them to react with one another, in a flow rate ratio of, as represented by molar ratio of the compounds in the solutions, from 1.00 to 1.35 of the basic alkali metal compound and from 0.60 to 40 of hydrogen peroxide or the metal peroxide per 1 of the perfluoroacyl halide, the yield of a perfluoroacyl peroxide based on the material perfluoroacyl halide can be remarkably improved as compared with conventional technique.