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碳—碳键新型引发剂的研究

STUDIES ON NEW TYPE CARBON-CARBON BOND INITIATORS

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【作者】 刘有成杨第伦吕惠临

【Author】 Liu Youcheng, Yang Dilun and Lu Huilin (Department of Chemistry, Lanzhou University,Lanzhou)

【机构】 兰州大学化学系兰州大学化学系

【摘要】 α-氰基苯乙酸乙酯用Cu++-TMEDA-O2进行氧化偶联反应,产物经色谱或重结晶法分离,经红外光谱、紫外光谱、1H核磁共振谱、质谱、元素分析鉴定及其碱性水解产物等认定为内消旋-2,3-二氰基-2,3-二苯基丁二酸二乙酯(Ⅰ).用Ⅰ引发苯乙烯进行本体聚合,测定了聚合温度和Ⅰ的用量对苯乙烯的转化率~时间曲线的影响,测定了各种条件下所得聚苯乙烯的分子量及其分散系数.1是一种既有效又安全的碳—碳键型引发剂.

【Abstract】 Diethyl 2,3-dicyano-2, 3-diphenylsuccinate (I) was synthesized by oxidative coupling" reaction of ethyl a-cyanophenylacetate with Cu ++-TMEDA-O3 system. The structure of I is determined on the basis of IR, 1HNMR, UV, MS and elemental analysis, and through alkaline hydrolysis of I to 2,3-diphenylsuccinonitrite. The configuration of I is identified to be the meso-isomer by x-ray crystallographic analysis in collaboration with the Institute of Physical Chemistry of Beijing University. The conversion-time curves are determined when I was used as initiator in the bulk polymerization of styrene at 80, 90,100, 110 and 120℃ respectively. Mw, Mn and dispersion coefficients of polymers obtained with a fixed amount of I as initiator in the bulk polymerization of styrene at 70, 80, 90, 100, 110, 120 and 150℃ or with various amounts of I as initiator at 100℃ are determined by GPC. The results show that I is a safe and efficient carbon-carbon bond initiator.

  • 【文献出处】 高等学校化学学报 ,Chemical Research In Chinese Universities , 编辑部邮箱 ,1984年03期
  • 【被引频次】30
  • 【下载频次】149
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