The invention relates to a preparation method of trifluoromethylsulfonyl
fluoride, which comprises the following steps: taking fluorosulfonyl
difluoroacetic acid, fluorosulfonyl difluoroacetate or fluorosulfonyl difluoroacetyl
fluoride as raw materials, and reacting with
fluorine gas to obtain the product trifluoromethylsulfonyl
fluoride. According to the method, the fluorosulfonyl
difluoroacetic acid (ester or acyl fluoride) directly reacts with the
fluorine gas, and complex multi-step reaction and separation and purification of intermediate products are not needed, so that the process flow is simplified, the production links are reduced, and the production efficiency is improved; the method has the advantages of low price of raw materials, mild
reaction conditions, low requirements on equipment, realization of
continuous production, and reduction of the equipment investment and the production cost; the preparation method is carried out under an
anhydrous condition, does not need to use any
organic solvent, and is environment-friendly and green; by controlling the
reaction conditions, the yield of the trifluoromethylsulfonyl fluoride can reach 85%, the purity of the trifluoromethylsulfonyl fluoride can reach 99.9%, the requirements of different fields for high-purity products can be met, and the method has a good industrial application prospect.