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采用改进的“一锅法”合成了N-正丁基硫代磷酰三胺(NBPT),以氨气替代传统液相试剂作为缚酸剂及后续胺化反应的原料,考察了反应温度、原料摩尔比、氨气流速、通氨间歇时间和胺化反应温度对产品收率的影响。优化的实验条件为:反应温度为0℃,正丁胺(0.42 mol)与三氯硫磷(0.35 mol)的摩尔比为1.2∶1,氨气流速为15 m L/min,通氨间歇时间为30 min,胺化反应温度为10℃。在该条件下,NBPT收率达75.6%,粗产物纯度为97%。采用红外光谱(IR)、元素分析、核磁分析(NMR)和液相色谱-质谱联用仪(LC-MS)对样品进行了表征。该合成过程具有操作步骤简单,生产成本低,副产物只有氯化铵等特点,是一条绿色合成路线。
N-n-butylthiophosphoric triamide (NBPT) was synthesized by a modified “one-pot method”. Ammonia instead of traditional liquid phase reagent was used as the acid-binding agent and the subsequent amination reaction. The effects of reaction Effect of temperature, raw material molar ratio, ammonia flow rate, ammonia breakthrough time and amination temperature on product yield. The optimum experimental conditions were as follows: the reaction temperature was 0 ℃, the molar ratio of n-butylamine (0.42 mol) to trichlorophosphine (0.35 mol) was 1.2:1, the flow rate of ammonia gas was 15 m L / min, For 30 min, the amination temperature is 10 ℃. Under these conditions, the NBPT yield was 75.6% and the crude product purity was 97%. The samples were characterized by infrared spectroscopy (IR), elemental analysis, nuclear magnetic resonance (NMR) and liquid chromatography - mass spectrometry (LC-MS). The synthesis process has the advantages of simple operation steps, low production cost and only by-products such as ammonium chloride, and is a green synthesis route.