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在线热裂解-气质联用分析缩合型和加成型硅橡胶

Analysis of Condensed and Addition Type of Silicon Rubbers by Online Pyrolysis Gas Chromatography-Mass Spectrometry

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【作者】 蒋可志倪勇邬继荣邱化玉来国桥

【Author】 JIANG Ke-Zhi,NI Yong,WU Ji-Rong,QIU Hua-Yu,LAI Guo-Qiao(Key Lab of Organosilicon Chemistry and Material Technology,Ministry of Education,Hangzhou Normal University,Hangzhou 310012)

【机构】 杭州师范学院有机硅化学及材料技术重点实验室

【摘要】 用在线热裂解-气质联用技术对缩合型硅橡胶和加成型硅橡胶分别进行分析,在其裂解产物中都检测到一系列的二甲基环硅氧烷环体。比较二者的裂解产物发现:缩合型硅橡胶非常容易发生裂解反应,产生低分子量的二甲基硅氧烷环体;而加成型硅橡胶相对难以裂解,有一定量的高级二甲基硅氧烷环体产生。除此之外还检测到微量的含氢环体和含乙烯基环体。这为缩合型和加成型这两种硅橡胶分析提供实验依据。

【Abstract】 All the online pyrolysis GC-MS experiments were carried out at pyrolyser (Pyprobe 5000,CDS Company,USA) and GC-MS(Trace 2000/DSQ,Thermofisher Company,USA). About 5 mg sample with some silica wool was uploaded into a silica pyrolysis tube,and the tube was introduced into the pyrolysis cell,which was remained at 270 ℃. The sample was pyrolyzed at 600 ℃ for 20 s,and the pyrolytic product was introduced into GC-MS for analysis. Both the condensed silicon rubbers and the addition type one gave a series of cyclicdimethylsilicon in the pyretic products. The results showed that silicon rubber of condensed type is more easily to occur decomposition and yields cyclicdimethylsilicon with lower molecular weight; whereas pyrolysis of the addition type silicon rubber can also produce higher cyclicdimethylsilicons,and trace hydrogen substituted cyclicdimethylsilicons and trace vinyl group substituted cyclicdimethylsilicons. The different Py-GC/MS behaviors give a chance to differentiate the type of silicone rubber.

【基金】 杭州市属高校重点实验室项目(No.0679XP11);杭州师范大学科研基金(No.2008XNM04)资助
  • 【文献出处】 分析化学 ,Chinese Journal of Analytical Chemistry , 编辑部邮箱 ,2009年04期
  • 【分类号】TQ333.93
  • 【被引频次】19
  • 【下载频次】498
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