当前位置: 首页 > 文章 > 亚氨基二乙腈合成双甘膦的工艺改进 农药 2017 (1) 14-17
Position: Home > Articles > Improved Synthesis of N-Phosphonomethylim Inodiacetic Acid by Iminodiacetonitrile Route Agrochemicals 2017 (1) 14-17

亚氨基二乙腈合成双甘膦的工艺改进

作  者:
窦艳容;李晋;郑幼松;胡健
单  位:
四川化工职业技术学院
关键词:
双甘膦;合成;工艺改进;亚氨基二乙腈
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。
译  名:
Improved Synthesis of N-Phosphonomethylim Inodiacetic Acid by Iminodiacetonitrile Route
作  者:
DOU Yan-rong;LI Jin;ZHENG You-song;HU Jian;Sichuan College of Chemical Technology;
关键词:
N-phosphonomethyl iminodiacetic acid;;synthesis;;process improvement;;iminodiacetonitrile
摘  要:
[Aims] The improved synthesis technology of N-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 p H 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 : sulfuric acid : phosphorus trichloride : formalin=1:30:0.3:1.25:1.45(mol), p H=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.

相似文章

计量
文章访问数: 17
HTML全文浏览量: 0
PDF下载量: 0

所属期刊

推荐期刊