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The synthesis novel technology of chlorocyclophosphazene

机译:氯环磷腈的合成新工艺

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The present paper provides a novel process for preparing chlorocyclophosphazene characterized by the combination of: (Ⅰ) The first step of reacting phosphorus pentachloride sublimated with ammonium chloride in an inert organic solvent(such as chlorobenzene) in the presence of N_2 and Zncl_2, and distilling off the solvent from the resulting reaction mixture to obtain a reaction product consisting essentially of chlorocyclophosphazene (up to 93%), and (Ⅱ) the second step of contacting a solution of the reaction product in the heptane with water in proption at temperature of about 60 ℃, separating the resulting aqueous layer from the organic layer, and isolating from the organic layer a mixture of chlorocyclophosphazene consisting essentially of the hexachlorocyclotriphosphazene which yield can reach up to 80%. Factors affecting on the process were also discussed in detail. The results show that the Technology is time saving(only 2.5 hours) under the suitable condition and the total fractional conversion is achieved 99%. The hexachlorocyclotriphosphazene were characterized by IR spectra,and the purity of product is over 98%.
机译:本文提供了一种新的制备氯环磷腈的方法,其特征在于:(Ⅰ)在惰性有机溶剂(如氯苯)中,在N_2和Zncl_2存在下,使升华的五氯化磷与氯化铵反应的第一步。从所得反应混合物中除去溶剂,得到基本上由氯环磷腈组成的反应产物(至多93%),(Ⅱ)第二步是使反应产物在庚烷中的溶液与水在约200℃的温度下接触。 60℃下,将所得水层与有机层分离,并从有机层中分离出基本上由六氯环三磷腈组成的氯环磷腈的混合物,其收率可高达80%。还详细讨论了影响该过程的因素。结果表明,在适当的条件下,该技术可节省时间(仅2.5小时),总转化率可达到99%。用红外光谱对六氯环三磷腈进行了表征,产品纯度达98%以上。

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