次磷酸化三(丙基醇)膦氢磷的合成及性能研究

Synthesis and properties of hypophosphorous tri(propyl alcohol) hydrogen phosphonium

以1-溴-3-甲氧基丙烷、三溴化磷为原料,制得三甲氧基丙基膦,再与次磷酸发生离子化反应,合成次磷酸化三(丙基醇)膦氢磷[(HOCH2CH2CH2)3PH]PO2H2.探讨了原料比、反应时间、反应温度对产率的影响,并通过TGA、元素分析、IR和UV可见光谱进行结构表征.研究了次磷酸化三(丙基醇)膦氢磷离子液体对羊毛织物的抗起毛起球性能.结果表明:1-溴-3-甲氧基丙烷、镁、三溴化磷和次磷酸的最佳物质的量比为3.2∶3∶2∶3;以氮气保护,冰水浴,格式反应和离子化反应的最佳反应时间均为1 h;次磷酸化三(丙基醇)膦氢磷产率为85.7%,羊毛织物的抗起毛起球性能达到4级.

The tri（methoxy propanol） phosphinegrignard was synthesized by 1-bromine-3-methoxy propane and phosphorus tribromide, and then reacted with hypophosphorous acid through ionization reaction to obtain hypophosphorous tri（propyl alcohol） hydrogen phosphonium. The effects of material ratio, reaction time and temperature on the yield were discussed. The structure of product was analyzed by thermogravimetric analysis （TGA）, element analysis, IR spectra and UV visible spectrum. The application performance of the product ionic liquid on the aspect of the antipilling of wool fabric was investigated. The results showed that the optimal molar ratio of 1-bromine-3-methoxy propane, magnesium, phosphorus tribromide and hypophosphorous acid was 3.2：3：2：3; nitrogen protection, ice water bath; the best response time of the preparation of grignard reaction and ionization reaction were 1 h, respectively. Under the optimum reaction conditions, the yield rate of the target product was 85.7% and the antipilling performance of the wool fabric was grade 4.