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苯氧基环磷腈合成处理方法的改进及表征

Post-treatment Improvement and Characterization of Phenoxy Cyclotriphosphazene Synthesis

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【作者】 薛宇鹏郝冬梅林倬仕陈涛尹亮陈崇伟王幸宜

【Author】 XUE Yu-peng1,2,HAO Dong-mei1,LIN Zhuo-shi1,CHEN Tao1,YIN Liang1,CHEN Chong-wei1,WANG Xing-yi2(1 Shanghai Research Institute of Chemical Industry,Shanghai 200062;2 East China University of Science and Technology,Shanghai 200237,China)

【机构】 上海化工研究院技术开发中心华东理工大学

【摘要】 苯氧基环三磷腈是一种重要的磷腈化合物,而苯氧基环磷腈(PCPZ)的制备会产生大量的副产物和过量的苯酚钠存在,使得合成实验的后处理较复杂且得很难得到纯度很高的产物。利用苯酚钠和六氯环三磷腈制备的苯氧基环三磷腈,根据产物易溶于四氢呋喃但难溶于水这一特点,找到了一种很简单的方法,使产物在大量水中结晶析出。这个方法操作方便,通过红外光谱、核磁共振、X衍射、高效液相色谱、热分析和凝胶渗透色谱表明得出的产物收率高于97%,纯度达100%,是一种很理想的后处理方法。

【Abstract】 Phenoxy cyclotriphosphazene was one of the most important phosphazene compounds,but for the existence of by-products and excessive sodium phenolate,the post-treatments for synthesis of phenoxy cyclotriphosphazene were complicated and it was hard to obtain products with high purity.Phenoxy cyclotriphosphazene was prepared with sodium phenolate and hexachlorocyclotriphosphazene.Since phenoxy cyclotriphosphazene could dissolve in THF,but could not in water.The product was poured into a beaker with a lot of water and phenoxy cyclotriphosphazene was precipitated.The product was analyzed by FTIR,NMR,XRD,HPLC,TGA,DSC and GPC.The yield was higher than 97% and the purity was 100%.

  • 【文献出处】 广州化工 ,Guangzhou Chemical Industry , 编辑部邮箱 ,2011年20期
  • 【分类号】TQ265.1
  • 【被引频次】8
  • 【下载频次】337
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