The influence of controllable main factors in the preparation of urea sulfate, as well as the crystal shape, X-ray diffraction pattern, hygroscopicity and acidity of the aqueous solution of the solid urea sulfate were studied. Experiments show that the main influencing factors in the preparation of urea sulfate are: the ratio of urea and sulfuric acid, reaction temperature and sulfuric acid concentration, among which n(urea)∶n(sulfuric acid)=2∶1, the reaction temperature is 80 °C, the mass fraction of sulfuric acid is 95%~98%, and its crystals are hexaprism under microscopy. The X-ray diffraction pattern showed that the X-ray diffraction pattern of the product and the possible generated substance was completely different, the hygroscopicity was linear with time, and the acidity of the aqueous solution was weaker than that of the same concentration of sulfuric acid and stronger than citric acid. Under the above reaction conditions, solid urea sulfate with stable properties and low cost can be prepared.