草甘膦的合成新工艺研究

A new process for synthesis of N-(phosphonomethyl) glycine

双氧水催化氧化法合成草甘膦具有后处理简单、收率高的特点,使该法成为一种重要的草甘磷合成工艺.以双甘膦为起始原料,经双氧水氧化,催化合成除草剂草甘膦,在合成草甘膦时,采用硫酸亚铁和盐A共同催化合成草甘膦反应结果理想.通过工艺优化,在反应温度71℃、双氧水滴加时间2 h、n(双甘膦)与n(双氧水)=1∶1.4,保温时间12 h、保温温度64℃等较佳工艺条件下反应总收率达85.9%,含量94.0%.草甘膦产品结构由IR,1HNMR确认.

The preparation of N-phosphonomethylglycine from N-phosphonomethyliminodiacetic acid by catalytic oxidation of hydrogen peroxide had some advantages such as simple post treatment and high yield. The best result was obtained when FeSO4 and A were used as the catalysts in the synthesis of N-phosphonomethylglycine. The optimal conditions were as follows： dropping temperature was 71 ℃ in 2 h, n（N-phosphonomethyliminodiacetic acid） ： n（hydrogen peroxide）=1 ： 1.4, then reacted at 64 ℃ for 12 h. The overall yield of N-（phosphonomethyl） glycine was 86.3% with 93% purity. The product was characterized by IR and 1^HNMR.