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4,4′-联苯-3,3′-二(2,4-戊二酮)的合成与热谱研究

Study on synthesis and thermograms of 3,3′-(biphenyl-4,4′-diyl)dipentane-2,4-dione

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【作者】 曾锦萍黄海平梅光泉于澍燕

【Author】 ZENG Jin-ping1,HUANG Hai-ping2,MEI Guang-quan*1,YU Shu-yan2 (1.Key Laboratory of Jiangxi University for Applied Chemistry and Chemical Biology,Yichun University,Yichun 336000,China;2.Department of Chemistry,Renmin University of China,Beijing 100872,China)

【机构】 宜春学院江西省高校应用化学与化学生物学重点实验室中国人民大学化学系

【摘要】 以4,4′-二(氯甲基)联苯和2,3-丁二酮-亚磷酸三甲酯(1∶1)加合物为原料合成了标题化合物,采用核磁共振谱、质谱、红外光谱和紫外可见光谱对化合物进行结构表征。在静态空气气氛中用热重-差示扫描量热分析法(TG-DSC)对其进行了热分析研究:168~436℃之间质量损失76.67%,最后的固体残留物为联苯骨架不完全燃烧的残留物。在272℃有一个放热峰,在210、302℃分别出现强吸热峰。结果表明该固态化合物在168℃以下很稳定。

【Abstract】 In this paper,3,3′-(biphenyl-4,4′-diyl)dipentane-2,4-dione was synthesized using 4,4′-bis(chloromethyl)biphenyl and 2,2,2-trimethoxy-4,5-dimethyl-1,3,2-dioxaphospholene as starting materials.Its molecule structure was characterized by 1HNMR,MS,IR and UV-Vis spectra.The thermal properties of 3,3′-(biphenyl-4,4′-diyl)dipentane-2,4-dione were studied based on the TG-DTG and DSC-DDSC analyses in a static air atmosphere.In a temperature range from 168 ℃ to 436 ℃,a mass loss of 76.67% was observed.The last solid residue was considered generally as the remnants of biphenyl skeleton after incomplete combustion.The maximum peak of heat release at 272 ℃ in DTG was resulted from exothermal decomposition reactions.The maximum peak of heat absorption at 210 ℃ and 302 ℃ in DSC was resulted from endothermic reactions,respectively.The test results showed the compound had higher thermal stability at 168 ℃.

【基金】 江西省自然科学基金项目(2008GZH0063);江西省教育厅科技项目(GJJ07429,GJJ09355)
  • 【分类号】O621.13
  • 【被引频次】4
  • 【下载频次】207
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