The invention discloses a preparation method of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide. The preparation method comprises a sulfonation reaction and a
dehydration condensation reaction, wherein in the sulfonation reaction,
methanesulfonic acid and a sulfonating agent are subjected to the sulfonation reaction, and
methylene disulfonic acid is obtained; in the
dehydration condensation reaction,
methylene disulfonic acid prepared by the sulfonation reaction and a
formaldehyde compound are dissolved in an
organic solvent and subjected to the
dehydration condensation reaction in the presence of adehydrating agent, a crude product of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide is produced and added to water to be washed, and a refined product of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide is obtained after
drying. According to the preparation method of 1,5,2,4-dioxadithiane 2,2,4,4-tetraoxide, the traditional method for obtaining intermediate
methylene disulfonic acid from
sodium methylene disulfonate as a
raw material by
precipitation, acidification and dehydration is abandoned, and methylene disulfonic acid is directly obtained from
methanesulfonic acid by sulfonation. The method has simple preparation process, high atom
utilization rate, little three-waste and high yield.