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    • 8. 发明公开
    • Process for manufacturing phosphorochloridothionates
    • 生产磷酰氯硫代磷酸酯的方法
    • EP0001687A1
    • 1979-05-02
    • EP78300433.6
    • 1978-09-29
    • STAUFFER CHEMICAL COMPANY
    • Mirviss, Stanley BurtonVon Lehman, Thomas Michael
    • C07F9/20
    • C07F9/20
    • In the production of phosphorodichloridothionates difficulties are encountered in purification, In the known processes many impurities result. A multi step process is provided which leads to a substantially pure product. This process comprises chlorinating bis(phosphorothioic)sulphides,thioic acids, or salts thereof, distilling the reaction mixtures, contacting the distillate with a thioic acid or salt thereof, contacting the mixture with water and distilling the organic material after the water contacting. In a representative example dimethyl phosphorochloridothionate is prepared from dimethyl phosphorodithioic acid by chlorination, distillation, reaction of the thionate distillate with dimethyl phosphorodithioc acid to produce a semi-pure thionate reaction mixture which is then contacted with water. The organic layer is then separated and distilled to product an over 99% pure product. The residue is recvcled for reaction with the thioic acid in the first step of the process.
    • 在二氯硫代磷酸酯的生产中,在纯化中遇到困难。在已知的方法中产生许多杂质。 提供了一个多步骤的过程,导致产品基本上纯净。 该方法包括氯化双(硫代磷酸)硫化物,硫代酸或其盐,蒸馏反应混合物,使馏出物与硫代酸或其盐接触,使该混合物与水接触并在与水接触后蒸馏有机物质。 在一个代表性实例中,二甲基磷酰氯硫代磷酸酯由二甲基二硫代磷酸通过氯化,蒸馏,硫酸盐馏出物与二甲基二硫代磷酸反应制备半硫酸盐反应混合物,然后与水接触。 然后将有机层分离并蒸馏以产生超过99%的纯产物。 在该方法的第一步骤中,将残留物与硫代酸进行回收。