脱水磷酰氯法合成磷酸二异辛酯

Synthesis of Diisooctyl Phosphate from Phosphenic Chloride

研究了脱水磷酰氯法合成磷酸二异辛酯的新方法。先以五氧化二磷和二氯亚砜反应制备了脱水磷酰氯,脱水磷酰氯再与异辛醇反应制得目标产物磷酸二异辛酯。考察了磷酰氯与异辛醇物质的量比、异辛醇的滴加温度、反应时间、反应温度和真空度等关键因素对反应的影响。实验结果表明,n(脱水磷酰氯)∶n(异辛醇)=1.0∶2.1、15℃下滴加异辛醇、60℃下反应3 h、真空度为0.08 MPa的条件下,磷酸二异辛酯的收率达96.2%,含量达97.9%。利用FT-IR和NMR对产物磷酸二异辛酯进行表征。

A novel process for the preparation of diisooctyl phosphate from phosphenic chloride was developed.Phosphenic chloride was synthesized from phosphorus pentoxide and thionyl chloride.Reaction of phosphenic chloride and isooctanol formed diisooctyl phosphate.The effects of key factors such as molecular ratio,dropping temperature of isooctanol,reaction time,reaction temperature and pressure on the reaction were investigated. The results indicated that under the optimal reaction conditions,n（ phosphenic chloride） ∶ n（ isooctanol） was 1. 0 ∶2. 1,isooctanol was dropped at 15 ℃,reaction time was 3 h at 60 ℃,and pressure was 0. 08 MPa,the yield of diisooctyl phosphate was 96. 2% with a purity of 97. 9%.The product diisooctyl phosphate was confirmed by FTIR and NMR.