The invention discloses a preparation method of vinyl
sulfate. The preparation method comprises the following steps: (1)
substitution reaction: carrying out
substitution reaction on
thionyl chloride and ethanediol used as raw materials, washing the reaction solution with deionized water to a
neutral state, standing, stratifying, and separating to obtain vinyl
sulfite; (2) oxidation reaction: adding
dichloromethane and a
ferric sulfate solution into the vinyl
sulfite, cooling to 0-5 DEG C, dropwisely adding a
sodium percarbonate solution to obtain a water-phase / organic-phase-coexistent reaction solution, standing the reaction solution, stratifying, separating out the water phase, and carrying out reduced pressure
distillation on the organic phase, thereby obtaining the vinyl
sulfate crude product; and refinement: recrystallizing the vinyl sulfate crude product by using
dichloromethane to obtain the high-purity vinyl sulfate. The preparation method has the characteristics of high mole yield, high product purity, low
moisture content, low
acid value and low preparation cost. The mole yield can reach 85% or above, the purity can reach 99% or above, the
moisture content is less than or equal to 60 ppm, and the
acid value is less than or equal to 60 ppm.