The invention discloses a preparation method of propylene hydroximic acid, wherein the temperature of the reaction is controlled by a thermostatic waterbath, a certain amount of
methyl acrylate and pure water are added into a reaction vessel, the quality of the pure water is 3-4 times that of the
methyl acrylate, the mixture is quickly stirred to enable the
methyl acrylate to be uniformly dispersed, then
hydroxylamine hydrochloride with the weight being 1.2-1.5 times that of the methyl
acrylate is added into a three-opening round bottomed flask, the mixture is constantly stirred to dissolve the mixture, when the
system temperature is kept stable at 20 DEG C, ionic membrane caustic soda liquid with the weight being equal to that of
hydroxylamine hydrochloride,is added into the mixture by using a dripping method so as to enable the reaction to perform smoothly, meanwhile, the temperature of a
reaction system is kept to be not more than 25 DEG C, low-pressure
distillation is performed after the reaction to remove dissociated unreacted
hydroxylamine and a by-product methyl
alcohol, cooling and suction
filtration are performed to remove the precipitated
salinity, and the final product is a water solution of propylene hydroximic acid. The reaction is controlled to be carried out slowly by adopting a method of dripping ionic membrane caustic soda liquid, so that the dissociated hydroxylamine is prevented from being decomposed and volatilized due to rapid
temperature increment, and the utilization ratio of raw materials is further improved.