万传玲-华理-保存条件对热解煤焦油中自由基检测的影响.pdfVIP

保存条件对热解煤焦油中自由基检测的影响 1 1* 1 1 2 2 2 万传玲 , 潘铁英 , 史新梅 , 周丽芳 , 刘瑞民 ,张德祥 , 高晋生 ( 1.华东理工大学分析测试中心,上海 200237 ; 2.华东理工大学资源与与环境工程学院,上海 200237) 摘 要:在用顺磁共振对中低阶煤热解煤焦油的研究中发现焦油中的自由基稳定性较差，不利 于检测工作的开展。为了提高热解煤焦油中自由基含量的检测精度，了解其样品最佳保存温 度与其自由基含量变化的原因，对不同保存温度和不同时间下的焦油样品进行了 EPR 测试 和 1H-NMR 测试。结果表明：保存温度越高，焦油中自由基含量增加趋势越明显；能够保 持热解煤焦油中自由基含量不变的最高温度约为-40℃以下。1H-NMR 结果显示导致热解煤 焦油中自由基含量增加的原因可能是焦油中结构单元之间的桥键断裂生成新的自由基所致。 关键词: EPR ；1H-NMR ；自由基； 煤焦油； 贮存温度 中图分类号：O652.1 Effects of Storage condition on Measuring Free Radicals in Pyrolysis Coal Tars 1 1 1 1 2 2 Chuanling Wan , Tieying Pan ,Xinmei Shi , Lifang Zhou , Ruimin Liu , Dexiang Zhang , 2 Jinsheng Gao ( 1 .East China University of Science and Technology, analysis and testing center, Shanghai 200237; 2. East China University of Science and Technology resources and environmental engineering college, Shanghai 200237) Abstract: The stability of free radicals in tars is relatively poor when researching low bank coal pyrolysis tars using EPR spectroscopy, which is bad for measuring work. Objective: To investigate the best preserving temperature of tars and the changing reason of free radicals. Method: EPR and 1 H-NMR analysis of different preserving temperatures and retention time tars. The results showed that free radicals concentration is being increased with the increasing of temperature; The highest preserving temperature to keep the free radicals concentration invariant may be below ﹣40 ℃. 1 H-NMR analysis shows that heteroatomic bond breaking may cause the increasing of free radicals.