中华医学超声杂志

应用化学 ›› 2010, Vol. 27 ›› Issue (11): 1276-1281.DOI: 10.3724/SP.J.1095.2010.00076

• 研究论文 • 上一篇    下一篇

金属醋酸盐催化合成聚丁二酸乙二醇酯预聚体和碳酸二甲酯

马楷1,2,刘绍英1*,姚洁1,王公应1   

  1. (1.中国科学院成都有机化学研究所 成都 610041；2.中国科学院研究生院 北京)
  • 收稿日期:2010-01-29 修回日期:2010-05-12 出版日期:2010-11-10 发布日期:2010-11-10
  • 通讯作者: 刘绍英, 研究员; E-mail:syliu@cioc.ac.cn; 研究方向：精细高分子合成与应用，清洁生产与催化剂

Simultaneous Synthesis of Poly(ethylene glycol succinate) Oligomers and Dimethyl Carbonate Using Metal Acetates as Catalysts

MA Kai1,2, LIU Shao-Ying1*, YAO Jie1, WANG Gong-Ying1   

  1. (1.Chengdu Institution of Organic Chemistry,Chinese Academy of Science,Chengdu 610041;
    2.Graduate School of Chinese Academy of Sciences,Beijing)
  • Received:2010-01-29 Revised:2010-05-12 Published:2010-11-10 Online:2010-11-10
  • Contact: Liu ShaoYing

PDF

1755

被引次数

12 | 7

摘要：

研究了醋酸盐催化碳酸乙烯酯（EC）和丁二酸二甲酯（DS）同时合成聚丁二酸乙二醇酯 (PES) 预聚体和碳酸二甲酯(DMC)的耦合反应新工艺。 采用气相色谱-质谱联用定性分析馏分组成；红外光谱、核磁共振表征了预聚物的结构；采用乌式粘度计测试了预聚物的特性粘数；气相色谱定量测定馏分碳酸二甲酯的收率以考察耦合反应的进度。 以对该反应催化效果最佳的无水醋酸锂为催化剂考察了物料配比、反应温度、反应时间、催化剂用量对耦合反应的影响，结果表明，最佳的工艺条件为：反应温度195～200 ℃，n(EC)∶n(DS)=2∶1，n(cat)∶n(EC+DS)=0.02∶1，反应时间为2 h，耦合反应所得的DMC收率为48.0%，聚丁二酸乙二醇酯预聚物的特性粘数为0.3787。

关键词: 金属醋酸盐, 聚丁二酸乙二醇酯, 酯交换, 碳酸乙烯酯, 丁二酸二甲酯, 碳酸二甲酯

Abstract:

Simultaneous synthesis of poly(ethylene glycol succinate) oligomers and dimethyl carbonate(DMC) was achieved by coupling reaction of ethylene carbonate(EC) and dimethyl succinate(DS) over various metal acetate catalysts. The effluent of coupling reaction was confirmed by GC-MS qualitative analysis. The structure of poly(ethylene glycol succinate) oligomeric product was characterized and assured by 1H NMR and FTIR spectra, and the intrinsic viscosity of poly(ethylene glycol succinate) oligomers was tested by the Ubbelohde type viscometer. The yield of DMC was gained by gas chromatography quantitative analysis, and the extent of coupling reaction could be calculated by the yield of DMC. Results showed that the lithium acetate has the highest catalytic activity. Using this compound as catalyst, the effects of experimental parameters including the molar ratio of EC to DS, reaction temperature, reaction time and amount of catalyst on the coupling reaction were investigated. The optimized reaction conditions are as follows: reaction temperature is in the range of 195 to 200 ℃, molar ratio of EC to DS is 2∶1, the molar fraction of catalyst is about 2%, reaction time is 2 h. Under these conditions, the yield of DMC was 48.0%; the intrinsic viscosity [η] of poly(ethylene glycol succinate) oligomers was 0.3787 dL/g.

Key words: metal acetate, Polyethylene glycol succinate, transesterification, ethylene carbonate, dimethyl succinate, dimethyl carbonate

中图分类号: 

网站版权 © 应用化学     本网站备案：吉ICP备12000082号