氨基苦味酸钠制备新技术研究

Study on New Manufacturing Technology for C_6H_2(NO_2)_2(NH_2)ONa

氨基苦味酸钠(简称钠盐)是制备DDNP的关键中间体,钠盐的结晶形貌和得率直接影响到DDNP的质量和得率。本文通过硫化钠直接还原苦味酸制得了利于重氮化反应的钠盐结晶。通过正交试验,考察了反应温度、硫化钠浓度、加料时间和搅拌速度对钠盐的影响。结果表明,制备钠盐的最佳条件为:反应温度55～60℃,硫化钠浓度12.5%,加料时间25min,搅拌速度155～160转/min。在此条件下,钠盐的得率提高了5%～10%,达到88%,DDNP得率提高了4%～8%。

C6H2（NO2）2（NH2）ONa is critical materials （or preparing DDNP,the crystalline shape and yield of C6H2（NO2）2 （NH2）ONa effect the quality and yield of DDNP. In this paper, C6H2（NO2）2（NH2）ONa crystalline was prepared by deoxidating picric acid with Na2S.The effect of reaction temperature, feed time, Na2S concenlration and mixing speed on C6H2（NO2）2（NH2） ONa was given by orthogonal test.The results show that the best manufactttring condition is reaction temperature of 55 - 60℃, Na2S concentration of 12.5%, feed time of 25min and mixing speed of 155 - 160rmp.Under the optimum condition, the yield of C6H2（NO2）2 （NH2）ONa and DDNP are increased 5% - 10% and 4% - 8% respectively.