The invention belongs to the technical field of
chemical engineering and fine
fluorine chemical synthesis, and particularly relates to a preparation method of
sulfuryl fluoride chloride. According to the preparation method, through the synergistic effect of a gas-liquid
reaction system and a closed-loop circulation
system, a
tertiary amine
hydrofluoric acid adduct (such as Et3N.nHF, n = 2-6) is used as a fluorinating
reagent,
sulfuryl fluoride chloride is generated through a rapid cross-flow reaction in excessive
sulfuryl chloride (SO2Cl2) under the conditions that the temperature is 65-100 DEG C and the pressure is 0.5-2.0 MPa, and a liquid-phase byproduct
tertiary amine
hydrochloride hydrogen fluoride adduct (such as Et3N.HCl. (n-1) HF) is used for preparing the
sulfuryl fluoride chloride. Supplementing
hydrogen fluoride to regenerate the catalyst and recycling; and after a gas-phase product is pressurized, rectified and purified by a light component removal
tower and a heavy component removal
tower, totally returning a light component (Cl2 / SO2) and a heavy component (SO2Cl2) to a
synthesis system for recycling. According to the method, the
reaction temperature, the reaction pressure, the
liquid phase dispersion degree and the
contact time are accurately controlled, so that the
reaction product generates SO2FCl with
high selectivity, and the byproduct (R3N.HCl. (n-1) HF) is kept in a
liquid phase, so that the reaction can be continuously carried out, and conditions are created for subsequent treatment.