The invention provides a preparation process of
trifluoromethyl sulfinyl
chloride. The preparation process comprises the steps as follows: 1) a synthesis kettle is taken, and
thionyl chloride is added; 2)
thionyl chloride is heated until
reflux and cooled to 0-5 DEG C, and
sodium trifluoromethanesulfinate is fed; 3) the temperature is increased to 15-20 DEG C,
distillation is performed, the steam is turned off and the temperature is reduced to 10 DEG C or lower when the temperature reaches 90-100 DEG C, and water is added to clean a
distillation kettle; 4) the material is distilled into a rectifying still, the rectifying still starts to heat up, front
cut fractions are collected after
reflux for 3-5 hours, whether the material in the
reflux pipe is transparent is observed when the temperature reaches 40-45 DEG C, and a finished product of
trifluoromethyl sulfinyl chloride is collected if the material is transparent, and reflux is continued if the material is not transparent; 5) the finished product is stopped from being collected when the temperature reaches 45-50 DEG C, reflux is continued, and the finished product of
trifluoromethyl sulfinyl chloride continues to be collected after the reflux temperature is reduced. The process is simple to operate, is green and has no
pollutant discharge during preparation, is energy-saving, consumption-reducing and good in economic benefit, an adopted
solvent is recyclable, obtained trifluoromethyl sulfinyl chloride has high purity and yield, and the production cost can be effectively reduced.