Abstract In order to solve problems in preparing tetraammine copper(Ⅱ) sulfate such as unreasonable dosage of reagent and ammonia pollution, this paper improved the experimental device, discussed the effect of concentration of cupric sulfate solution and aqueous ammonia on the yield, determined the suitable dosage of ammonia and ethanol, analyzed the washing effect of some washing detergents, and recycled the residual ethanol in the filtrate. The optimized condition for preparing tetraammine copper(Ⅱ) sulfate was: 0.5~1.0 mol/L cupric sulfate solution reacting with 4~8 mol/L aqueous ammonia with an excess of 80%, and the dosage of ethanol is 3 times of the volume of the reaction mixture.