The invention relates to a novel method for preparing dihydroxyurea and belongs to the field of
organic synthesis. The dihydroxyurea belongs to a novel salt-free
reducing agent which is used for spent fuel
post treatment and has good application prospects. The novel method is mainly characterized in that under the
anhydrous conditions,
solid phosgene and
hydroxylamine are used for synthesizing the dihydroxyurea. Concretely,
hydroxylamine and
potassium acetate are firstly placed into a three-opening flask, are placed into an ice
salt bath and are stirred into
emulsion. In addition, the
solid phosgene is dissolved into 1, 4-dioxane, the mixed liquid is placed into a constant-pressure liquid dripping funnel, when the temperature is below 0 DEG C, the
solid phosgene mixing liquid is dripped into the
emulsion at the controlled speed, and the temperature is maintained at 0 to 5 DEG C. The reaction is continuously carried out for 2 hours after the dripping completion, and then, the pH of the solution is regulated to 2 to 3 through concentrated
hydrochloric acid.
Solid materials are removed through filtering, solvents are removed through rotary
evaporation on filter liquid, and solid is obtained. A proper amount of
tetrahydrofuran is used for extracting the dihydroxyurea in the solid, the solvents are removed through the rotary
evaporation, coarse dihydroxyurea is obtained,
ethanol is used for recrystallization, and the pure dihydroxyurea is obtained. Through the detection and characterization on products by various methods, the product purity is 95 percent, and the yield is 57 percent.