Research On Synthesis Of Diacetylmonoxime And Its Derivative Hydroxylamine Hydrochloride

Oxime is an important chemical product, which can be used as oxygen eliminating agent, anti-skinning agent and the raw material to prepare crosslinking agent. Of all the method of preparing oxime, the ammoxidation of ketone is a clean and atom economic way. Highly efficient and low costing ammoxidation is attracting more and more academic attention. The author presented the preparation of hydroxylamine chloride from butanone, ammonia and hydrogen peroxide. The effect of reaction conditions, including molar ratio, time and temperature, on the yield of diacetylmonoxime were investigated. And the optimum reaction conditions were obtained, which are:n(butanone):(H2O2):n(NH3)=1:1:1.7, temperature (65℃), time (1h), and the yield of diacetylmonoxime is92.0%.Hydroxylamine chloride is and important chemical material and intermediate, which is widely used in chemical industry. Preparing hydroxylamine chloride from oxime is an convenient reaction with simple separation, and the cost is low. So it is available for industrial amplification. The author performed the comparison of different oximes in the preparation of hydroxylamine chloride, which gave the preferable one, diacetylmonoxime. Subsequently, the effect of reaction conditions on the yield of hydroxylamine chloride was investigated, and the optimum reaction conditions were obtained as:n(diacetylmonoxime):n(HCl)=1:1.2, temperature (100℃), time (80min), and the yield of hydroxylamine chloride is90.0%.A industrial production of diacetylmonoxime was designed with output of3000t/a based on the experiment of synthesis of diacetylmonoxime. With utilization of the current DCS system, the production proceeds stablely. The author also made a manipulation instruction for the production process.