【摘要】 针对3-硝基-1,2,4-三唑-5-酮(NTO)硝化过程中产生大量废酸导致"三废"综合治理成本高的问题,通过向废酸中补加少量工业浓硝酸制成质量分数为70%的硝酸溶液作为硝化剂,硝化1,2,4-三唑-5-酮(TO),循环合成目标化合物NTO。采用红外光谱、核磁共振光谱、元素分析对其进行了结构表征。考察了硝化剂用量、反应时间、反应温度对产品的影响,优化了硝化反应条件,确定硝化的最佳反应条件为:n(TO)n(HNO3)=16,反应温度60～65℃,反应时间1 h,纯度可达99.9%。废酸循环利用10次以上,平均收率82%,硝酸用量减少了67.6%。更多还原

【Abstract】 In order to solve the problem of high cost and pollution for treatment of a large quantity of nitric acid in the nitration of 3-nitro-1,2,4-triazol-5-one(NTO),the nitration agent(70% nitric acid),which was designed and prepared by the addition of an appropriate amount of industrial nitric acid into waste acids,was used to synthesize NTO from 1,2,4-triazol-5-one with an average yield of 82% and purity of 99.9%.The products were characterized by IR,13C NMR,1H NMR,MS and elemental analysis etc.The effects of various factors such as temperature and reaction time etc.on the yield of the nitration reaction were studied.It was experimentally found that the conditions of nitration reaction were optimized as: molar ratio of TO/HNO3 1/6,nitration temperature 60-65 ℃,reaction time 1 h.the new nitration agent(70% nitric acid)can be reused for ten times and the amount for the addition of nitric acid reduces by 67.6%.更多还原