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HBIW中主要杂质的鉴定及形成途径

Identification and Forming Process of Main Impurity in HBIW

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【作者】 陈华雄陈树森李丽洁史彦山杨荣杰向玉联

【Author】 CHEN Hua-xiong1,CHEN Shu-sen1,LI Li-jie1,SHI Yan-shan1,YANG Rong-jie1,XIANG Yu-lian2 (1.School of Material Science and Engineering,Beijing Institute of Technology,Beijing 100081,China;2.Institute of Chemical Defence,PLA,Beijing 102205,China)

【机构】 北京理工大学材料科学与工程学院解放军防化指挥工程学院 北京100081北京100081北京102205

【摘要】 采用常压制备色谱分离了六苄基六氮杂异伍兹烷(HBIW)中提取的杂质,重结晶得到其中一种主要的杂质晶体;应用FT-IR1、H-NMR、ESI-MS、元素分析鉴定了该杂质的结构,研究了它的形成途径及对氢解反应催化剂钯的影响。结果表明HBIW中的主要杂质是草酰二苄胺(Bn—NHCO-)-2,它主要由醛胺缩合中间体C6H5CH2NHCH(OH)CH(OH)NHCH2C6H5在空气中氧化而生成,氢解反应中它会危害到催化剂钯的活性。

【Abstract】 The impurities in hexabenzylhexaazaisowurtzitane(HBIW) were isolated by preparative chromatograph,and the crystal of the main impurity in HBIW was obtained by recrystal technic.The structure of the impurity was studied with FT-IR,1H-NMR,ESI-MS,element analysis.The forming of the impurity and its effect on the catalyst Pd in the hydrogenolysis are discussed.The results show that the main impurity in HBIW is oxalic dibenzylamine(Bn—NHCO-)-2,which is formed from C6H5CH2NHCH(OH)CH(OH)NHCH2C6H5 oxidated by the oxygen in the air.

  • 【分类号】TQ560.7
  • 【被引频次】5
  • 【下载频次】251
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