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Microwave-accelerated synthesis of tributyl citrate using ionic liquid as catalyst and investigation of its properties

XIA Haihong,JIANG Jianchun,XU Junming,LI Jing,LIU Peng   

  1. Institute of Chemical Industry of Forest Products,Chinese Academy of Forestry,Nanjing 210042,Jiangsu,China
  • Online:2014-04-05 Published:2014-04-05

微波加热促进离子液体催化合成柠檬酸三丁酯及其性能

夏海虹,蒋剑春,徐俊明,李静,刘朋   

  1. 中国林业科学研究院林产化学工业研究所,江苏 南京 210042

Abstract: Imidazole acid ionic liquid was prepared and used in synthesis of tributyl citrate. By microwave heating,reaction time could be shortened from 4 h to 0.5 h. Experiments showed that the optimum conditions using [HSO3-pmim]+[HSO4]? as catalyst by microwave heating were as follows:mole ratio of butanol to citric acid was 6∶1,the dosage of catalyst was 15% based on citric acid,microwave irradiation power was 650W,reaction time was 0.5 h,and carboxyl conversion rate was 99%. The catalyst could be reused 7 times without treatment,and carboxyl conversion rate was still more than 96%. Plasticizing performance tests showed that with addition of 15% TBC,tensile strength decreased to 35.19 MPa,compression strength decreased to 57.35 MPa,bending strength decreased to 70.61 MPa,and shear strength increased to 11.94 MPa. So tributyl citrate would take better replacement of DOP.

Key words: microwave, ionic liquids, esterification, catalyst, tributyl citrate, plasticizing performance

摘要: 制备了咪唑类酸性离子液体,用于催化合成柠檬酸三丁酯,使用微波加热可使反应时间由4 h缩短至0.5 h。通过试验得出,在微波加热方式下[HSO3-pmim]+[HSO4]?催化的最佳反应条件为:醇酸比为6∶1,催化剂用量为柠檬酸质量的15%,微波辐射功率为650 W,反应时间为0.5 h,羧基转化率可达99%。反应过的催化剂不经任何处理可重复使用7次,转化率仍在96%以上。增塑性能测试表明,添加15%的TBC,拉伸强度降至35.19 MPa,压缩强度降至57.35 MPa,弯曲强度降至70.61 MPa,拉伸剪切强度增至11.94 MPa,说明柠檬酸三丁酯可以作为邻苯二甲酸酯类增塑剂的良好替代品。

关键词: 微波, 离子液体, 酯化, 催化剂, 柠檬酸三丁酯, 增塑性能

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