Synthesis and Preparation of Methyl Hypophosphate and Analysis Method by Ion Chromatography
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 Na2CO3 and 1.0 mmol/L NaHCO3 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.
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