亚氨基二乙腈合成双甘膦的工艺改进  

Improved Synthesis of N-Phosphonomethylim Inodiacetic Acid by Iminodiacetonitrile Route

作　　者：窦艳容 李晋[1] 郑幼松[1] 胡健[1] 

机构地区：[1]四川化工职业技术学院,四川泸州646005

出　　处：《农药》2017年第1期14-17,共4页Agrochemicals

基　　金：四川省泸州市重点科研基金项目[2013-S-43(4/5)]

摘　　要：[目的]亚氨基二乙腈法合成双甘膦,为了提高产品收率,在亚氨基二乙腈直接酸解时加入硫酸溶液。[方法]以亚氨基二乙腈为原料,在水溶液中滴加三氯化磷和硫酸酸解、缩合制得双甘膦。考察了三氯化磷、甲醛、硫酸用量及p H终点值对双甘膦收率的影响。[结果]酸解反应中加入硫酸,增强反应体系的酸性强度,提高反应温度,双甘膦收率达94%。[结论]确定最佳的工艺条件为亚氨基二乙腈、水、硫酸、三氯化磷、甲醛的摩尔比为1∶30∶0.3∶1.25∶1.45,中和反应终点控制p H值为1.0。在该条件下,双甘膦收率94%以上,纯度98%以上。用液相色谱和核磁共振对双甘膦进行表征。[Aims] The improved synthesis technology ofN-phosphonomethyl iminodiacetic acid was investigated by the addition of sulfuric acid in this paper. [Methods] It was prepared by iminodiacetonitrile, phosphorus trichloride and sulfuric acid. Influence of dosage of material ratio and pH on the reaction is investigated. [Results] Total yield of N-phosphonomethyl iminodiacetic acid was 94% under optimized conditions. [Conclusions] The optimum technology conditions were iminodiacetonitrile： water： sulfiuic acid： phosphorus trichloride： formalin= 1：30：0.3：1.25：1.45 （mol）, pH= 1. The total yield of N-phosphonomethyl iminodiacetic acid was up to 94%, and the purity 98%. The product was confirmed by means of HPLC and 1H NMR technique.

关 键 词：双甘膦 合成 工艺改进 亚氨基二乙腈 

分 类 号：TQ457.2[化学工程—农药化工]