The invention belongs to the technical field of acyclic compounds, and particularly relates to a preparation method of tert-amyl peroxyacetate. Adding a tert-amyl
hydrogen peroxide aqueous solution into a
solvent, and stirring to obtain a
mixed solution; under the stirring condition, p-toluenesulfonic acid and
iron phosphide are sequentially added into the
mixed solution, stirring reaction continues after adding is completed, and reaction liquid I is obtained; under the stirring condition,
acetic anhydride is added into the reaction liquid I, stirring reaction continues after adding is completed, and reaction liquid II is obtained; adding a washing liquid into the reaction liquid II, stirring, washing, and separating to obtain a tert-amyl peroxyacetate crude product; and washing and
drying the tert-amyl peroxyacetate crude product, and removing the
solvent to obtain the tert-amyl peroxyacetate. The method avoids the problems of a large amount of
hydrochloric acid generated by a traditional
acyl chloride method and corrosivity caused by using
sulfuric acid as a catalyst; meanwhile,
iron phosphide has
magnetism, cyclic utilization can be achieved through
magnetic separation after the reaction is finished, p-toluenesulfonic acid can be regenerated through
ion exchange resin, and the production cost is greatly reduced.