环己酮肟水解法合成硫酸羟胺的反应新工艺

摘要

为了开发一种合成硫酸羟胺的新工艺,以氯化铵作氮源合成的环己酮肟为原料,硫酸为催化剂,考察了不同反应条件下环己酮肟水解合成硫酸羟胺反应的性能,并采用红外光谱分析、元素分析和熔点分析对硫酸羟胺固体产品进行了表征分析确定.结果表明:当环己酮肟88.5 mmol,去离子水、硫酸和环己酮肟的物质的量之比为12.55:1.87:1,60 ℃下反应1 h,环己酮肟的转化率接近100%,硫酸羟胺固体产品的收率为41.7%.在此基础上,借助环己酮和环己酮肟的相互转化,构建了以低附加值氯化铵制备羟胺盐的新工艺过程.该过程不仅提供了合成固体羟胺盐的新工艺,而且为氯化铵废料的资源利用提供了良好的借鉴.%In order to develop a novel process for the synthesis of hydroxylamine sulfate, cyclohexanone oxime synthesized with ammonium chloride as nitrogen source was used as a raw material, and sulfuric acid was used as a catalyst to examine the performance of the synthesis of hydroxylamine sulfate by hydrolysis of cyclohexanone oxime under different reaction conditions. The hydroxylamine sulfate solid product was characterized and analyzed by infrared spectroscopy, elemental analysis and melting point analysis. The results showed that when cyclohexanone oxime was 88.5 mmol, the ratio of the deionized water, sulfuric acid, and cyclohexanone oxime was 12.55:1.87:1, and the reaction was conducted at 60 °C for 1 h, the conversion of cyclohexanone oxime was close to 100%, and the yield of hydroxylamine sulfate solid product was 41.7%. Based on these results, a new process for the preparation of hydroxylamine salts with low added value ammonium chloride was constructed with the aid of the mutual conversion of cyclohexanone and cyclohexanone oxime. This process not only provided a new process for the synthesis of solid hydroxylamine salts, but also provided a good reference for the resource utilization of ammonium chloride waste.