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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%。
Sodium picrate (referred to as sodium salt) is a key intermediate for the preparation of DDNP. The crystalline morphology and yield of sodium salt directly affect the quality and yield of DDNP. In this paper, direct sodium sulfide reduction of picric acid obtained diazotization reaction of sodium salt crystallization. Through orthogonal experiment, the effects of reaction temperature, sodium sulfide concentration, feeding time and stirring speed on sodium salt were investigated. The results showed that the optimum conditions for the preparation of sodium salt were: reaction temperature 55 ~ 60 ℃, sodium sulfide concentration 12.5%, feeding time 25min, stirring speed 155 ~ 160 rev / min. Under these conditions, the yield of sodium salt increased by 5% -10% to 88%, and the yield of DDNP increased by 4% -8%.