One Pot, One Feeding Step, Two-Stage Polymerization Synthesis and Characterization of (PTT-b-PTMO-b-PTT)n Multiblock Copolymers
One Pot, One Feeding Step, Two-Stage Polymerization Synthesis and Characterization of (PTT-b-PTMO-b-PTT)n Multiblock Copolymers
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DOI：
10.1021/ma400969a
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发表时间：
2013-09
期刊：
影响因子：
5.5
通讯作者：
Qiaozhen Xu;Jianying Chen;Weichun Huang;T. Qu;Xiaohong Li;Yaowen Li;Xiaoming Yang;Y. Tu
中科院分区：
文献类型：
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作者：
Qiaozhen Xu;Jianying Chen;Weichun Huang;T. Qu;Xiaohong Li;Yaowen Li;Xiaoming Yang;Y. Tu
采用PTMO大分子引发剂熔融聚合环状低聚对苯二甲酸丙二醇酯（COTT），一锅法一步合成了聚对苯二甲酸丙二醇酯-聚四氢呋喃（PTT-b-PTMO-b-PTT）n。采用改进的1HNMR定量表征技术，通过对聚合物链端结构和官能团的分析，研究了不同反应时间下聚合物的结构。结果表明，该共聚物的聚合动力学为两阶段聚合机理：第一阶段为PTMO大分子引发剂引发环状低聚对苯二甲酸丙二醇酯（COTTs）熔融开环聚合，形成三嵌段共聚物;第二阶段为嵌段共聚物的原位缩聚，形成多嵌段共聚物。凝胶渗透色谱（GPC）和粘度实验进一步证实了这一点。据我们所知，这是第一个报告的聚醚酯分子。
We present here the one pot, one step synthesis of poly(trimethylene terephthalate)-block-poly(tetramethylene oxide) multiblock copolymers (PTT-b-PTMO-b-PTT)n by melt polymerization of cyclic oligo(trimethylene terephthalate)s (COTTs) with PTMO macroinitiator. An improved quantitative 1H NMR characterization technique was developed and applied to investigate the multiblock copolymers’ structure with different reaction time by the chain end and functional groups estimation. The polymerization kinetics was revealed, and the results indicated a two-stage polymerization mechanism: melt ring-opening polymerization of cyclic oligo(trimethylene terephthalate)s (COTTs) by PTMO macroinitiator to form triblock copolymers at first stage, followed by the in-situ condensation polymerization of block copolymers to produce multiblock copolymers at second stage. This was further confirmed by the gel permeation chromatography (GPC) and viscosity experiments. To our knowledge, this is the first reported poly(ether ester) m...