A raw material is provided which permits preparation of tetrakis[tris(dimetHylamino)phosphoranylideneamino]phosphonium hydroxide by an extremely simple process.
The raw material, [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylidene amino]phosphonium dichloride is prepared by bringing hydrogen chloride into contact with tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride and adding the former on the latter. Tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium hydroxide is prepared by bringing an aqueous solution of the dichoride into contact with an OH--form ion exchange resin.
A separation process, is provided in which tetrakis[tris(dimethylamino)phosphoranylideneamino]phosphonium chloride is separated from solution by extracting it out, as [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylidene amino]phosphonium dichloride, into a water phase.
An isolation process is also provided, in which an aqueous solution of [tris(dimethylamino)phosphonioamino]tris[tris(dimethylamino)phosphoranylidene amino]phosphonium dichloride is neutralized so that tetrakis[tris(dimethylamino)phosphoranylideneamino]phosph onium chloride is regenerated and precipitated as a solid.
本发明提供了一种原材料,可通过极其简单的工艺制备四[三(
二甲氨基)亚
磷酰
氨基]氢氧化
鏻。
原材料[三(二甲基
氨基)
磷酰
氨基]三[三(二甲基
氨基)
磷酰亚
氨基]二
氯化
鏻是通过
氯化氢与四[三(二甲基
氨基)
磷酰亚
氨基]
氯化
鏻接触并在后者上加入前者而制备的。四[三(二甲基
氨基)
磷酰亚
氨基]氢氧化
鏻是通过将二
氯化碳
水溶液与 OH 型离子交换
树脂接触而制备的。
提供了一种分离工艺,将四[三(二甲基
氨基)亚
磷酰
氨基]
氯化
鏻从溶液中分离出来,将其作为[三(二甲基
氨基)亚
磷酰
氨基]三[三(二甲基
氨基)亚
磷酰
氨基]二
氯化
鏻萃取到
水相中。
还提供了一种分离工艺,在该工艺中,[三(二甲基
氨基)膦酰
氨基]三[三(二甲基
氨基)
磷酰亚
氨基]二
氯化
鏻的
水溶液被中和,从而使四[三(二甲基
氨基)
磷酰亚
氨基]
氯化
鏻再生并沉淀为固体。