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钛络合物均相催化合成聚六氢苯酐二甘醇酯

蒋平平1,2,沈敏亮1,董玉明1,张晓鸣2,冯 骉2   

  1. (1江南大学化学与材料工程学院;2食品科学与技术国家重点实验室,江苏 无锡 214122)
  • 出版日期:2011-03-05 发布日期:2011-03-05

Synthesis of polydiglycol cyclohexane 1,2-dicarboxylate catalyzed by titanium complex

JIANG Pingping1,2,SHEN Minliang1,DONG Yuming1,ZHANG Xiaoming2,FENG Biao2   

  1. (1School of Chemical and Material Engineering,Jiangnan University;2State Key Laboratory of Food Science and Technology,Jiangnan University,Wuxi 214122,Jiangsu,China)
  • Online:2011-03-05 Published:2011-03-05

摘要:

以六氢苯酐和二甘醇为原料,钛络合物钛酸正四丁酯为催化剂合成聚六氢苯酐二甘醇酯。结果表明,钛酸正四丁酯催化合成聚六氢苯酐二甘醇酯的最佳反应条件为:醇酸摩尔比为1.1∶1,催化剂用量为0.8%(以六氢苯酐质量计),反应温度为220 ℃,反应时间为5 h,-0.095 MPa压强下减压时间为2.5 h,减压温度为220 ℃,酯化率大于99.0%。合成产物聚六氢苯酐二甘醇酯的数均分子量Mn为14000,重均分子量Mw为15000,分子量具有窄分布物性。

Abstract:

Poly diglycol cyclohexane 1,2-dicarboxylate was prepared from hexahydrophthalic anhydride and diethylene glycol,catalyzed by titanium complex tetrabutyl titanate. The best reaction conditions of esterification were determined as follows:molar ratio of diethylene glycol to hexahydrophthalic anhydride 1.1∶1,amount of catalyst 0.8%(based on the mass of hexahydrophthalic anhydride),reaction temperature 220 ℃,reaction time 5 h,vacuum reaction time 2.5 h,vacuum reaction temperature 220 ℃ under vacuum(-0.095 MPa),and esterification yield could be up to 99.0%. Number-average molecular weight of the product poly diglycol cyclohexane 1,2-dicarboxylate was 14000,and weight-average molecular weight of the product was 15000. Molecular weight distribution of the product was narrow.

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