The invention provides a preparation method of hexafluorobutadiene, which comprises the following steps: 1) carrying out
electrophilic addition reaction on
chlorotrifluoroethylene and liquid
bromine at normal temperature and normal pressure to generate 1, 2-dibromo-1-chloro-1, 2, 2-
trifluoroethane; 2) mixing
zinc powder, 1, 2-dibromo-1-chloro-1, 2, 2-
trifluoroethane and an aprotic polar
solvent, and carrying out a reaction so as to obtain a
zinc reagent containing 1-chloro-2-bromo-1, 2, 2-trifluoroethyl
zinc bromide and 1, 2-dibromo-1, 2, 2-trifluoroethyl zinc
chloride; 3) adding a catalyst and a zinc
reagent, and carrying out a self-
coupling reaction to generate an
intermediate product containing 1, 4-dibromo-2, 3-dichloro-1, 1, 2, 3, 4, 4-hexafluorobutane and 1, 2, 3, 4-tetrabromo-1, 1, 2, 3, 4, 4-hexafluorobutane; 4) dehalogenating the
intermediate product to generate hexafluorobutadiene; the method has the effects of simple reaction process, relatively low risk, relatively mild
reaction conditions and relatively high yield.