甲基次膦酸合成制备以及离子色谱分析方法

Synthesis and Preparation of Methyl Hypophosphate and Analysis Method by Ion Chromatography

开发一种甲基次膦酸的合成制备方法,并采用离子色谱及电导检测的方法对甲基次膦酸进行检测。在制备过程中,以甲基亚膦酸二乙酯为反应原料,一次水解得到甲基亚膦酸单乙酯,二次水解得到甲基次膦酸。分离提纯得到甲基次膦酸纯品,建立离子色谱检测方法,采用阴离子柱以3.2 mmol/L Na_(2)CO_(3)和1.0 mmol/L NaHCO_(3)为淋洗液,流速0.7 mL/min淋洗,抑制电导检测。在选定的离子色谱条件下,方法的标准偏差为0.24,变异系数为0.25%,回收率为98.92%,适用于甲基次膦酸的分析。利用检测方法跟踪整个草铵膦生产工艺中产生过程和最终去向,对于优化草铵膦生产工艺具有重要意义。

A method of synthesis and preparation of methylphosphonic acid was developed,and the method of ion chromatography and conductance detection was used to detect methylphosphonic acid.In the preparation process,diethyl methylphosphite was used as the reaction material to obtain monoethyl methylphosphite by one hydrolysis and methyl hypophosphate by two hydrolysis.The pure methylhypophosphate product was separated and purified,and an ion chromatography method was established.3.2 mmol/L Na_(2)CO_(3)and 1.0 mmol/L NaHCO_(3)were used as leachate by anion column at the flow rate of 0.7 mL/min,and the conductivity detection was inhibited.The standard deviation of the method is 0.24,the coefficient of variation is 0.25%,and the recovery is 98.92%,which is suitable for the analysis of methylphosphonic acid under the selected ion chromatography conditions.It is of great significance to optimize the production process of phosphine oxalate by using detection method to track the production process and final destination of the whole production process.