The invention relates to a preparation method of vinyl
sulfate. The preparation method comprises the following steps: adding
ethylene glycol into a reaction kettle A filled with a
halohydrocarbon solvent, uniformly stirring, dropwise adding
thionyl chloride to carry out a
substitution reaction, removing
hydrogen chloride by reduced-pressure
distillation, then, washing a reaction solution to be neutral by using a saturated
sodium bicarbonate solution, standing still, and skimming to obtain a glycol
sulfite halohydrocarbon solution; adding the glycol
sulfite halohydrocarbon solution into a reaction kettle B, adding
monopotassium phosphate or
sodium tungstate as a catalyst, regulating the pH by using a
sodium bicarbonate aqueous solution, and adding a
sodium hypochlorite aqueous solution to carry out an oxidation reaction; at the end of the reaction, skimming to obtain a vinyl
sulfate halogenated
alkane solution, carrying out concentration, then, adding n-
hexane to carry out recrystallization, and carrying out
filtration to obtain high-purity vinyl
sulfate. By using the preparation method, raw materials are available, the price of the catalyst is low, the product is easy to purify, and the obtained product is low in acidity, low in
water content, high in purity and suitable for large-scale production.