Preparation Of Solid Hydroxylamine Sulphatethe And Hydroxylamine Hydrochloride

Using low-concentration hydroxylamine sulphate as raw material, this article measures the precipitation curves of both ammonium sulfate and hydroxylamine sulphate, carries out the research of the preparation of solid hydroxylamine sulphatethe using liquidating method and the preparation of solid hydroxylamine hydrochloride using butanone oximation hydrolyzing method. The precipitation curve shows that the deposition fraction (f) of (HONH₃)₂ .S0₄ and (NH,) ..SO., increases with the increase of the methanol/ water ratio(V). With the increase of V, f increases rapidly when V < 2. 0, while the increase of f is not apparent when V > 2. 0. When V = 2. 0, the deposition fraction (f ) for (HOMO 2SO4 is 0.992 while that for (NH4) 2S04 is 0.9802. The influences of factors such as volume of methanol and ammonia water, reaction temperature, reaction time and pH value on the yield and purity of hydroxylamine sulphate are studied in the preparation of solid hydroxylamine sulphate using liquidating method. The optimized conditions are obtained as follows: the volumes of low-concentration hydroxylamine sulphate, methanol and ammonia water are 50ml, 110. 0ml and 18.0ml, respectively, reaction time is 45 min, reaction temperature is 40 , pH value is 5.4. Under the above conditions, the yield of hydroxylamine sulphate is 81.0% with purity of 99.0%. In the research of the preparation of solid hydroxylamine hydrochloride using butanone oximation hydrolyzing method, the influences of acetoxime, 2-butanoneoxime and cyclohexanone oxime on the yield of the product are compared and 2-butanoneoxime is chosen for the detailed study. The influences of C,H9NO/HC1 molar ratio, reaction temperature and reaction time on the yield of hydroxylamine sulphate are studied. It is found that the yield of around 73.0% is achieved underthe molar ratio of 1-1. 5, reaction temperature of 100°C and reaction time of 1-1.5 hours. In the synthesis of 2-butanoneoxime, the influences of total molar ratio of 2-butanone and hydroxylamine sulphate, reaction temperature and reaction time on 2-butanoneoxime are studied. Under total molar ratio of 1: 1, reaction temperature of 48⁵2°C and reaction time of 1 h, the yield can be over 90%.Based on the results on the preparation of 2-butanoneoxime and the real condition of Juhua Nylon Plant, a concept design is worked out for the production of 2-butanoneoxime with an annual capacity of 3000 tons. The design adopts a double-section backwash oximation, stream stripping reclaimation, and film evaporation process. The design also takes advantage of the existing DCS system in Juhua Nylon Plant to stabilize the operation. An operation manual for the production of 2-butanoneoxime is also compiled by referring to the experience in cyclohexanone production.