From miscible to partially miscible biodegradable double crystalline poly(ethylene succinate)-b-poly(butylene succinate) multiblock copolymers
From miscible to partially miscible biodegradable double crystalline poly(ethylene succinate)-b-poly(butylene succinate) multiblock copolymers
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DOI：
10.1039/c1py00456e
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发表时间：
2012-01
影响因子：
4.6
通讯作者：
J. Zeng;Qun-Ying Zhu;Xi Lu;Yiyong He;Yu-Zhong Wang
中科院分区：
文献类型：
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作者：
J. Zeng;Qun-Ying Zhu;Xi Lu;Yiyong He;Yu-Zhong Wang
以1，6-六亚甲基二异氰酸酯(HDI)为扩链剂，通过二羟基聚丁二酸乙二醇酯(HO-PES-OH)和聚丁二酸丁二醇酯(HO-PBS-OH)的扩链反应，成功合成了一系列具有不同PES和PBS嵌段长度的可生物降解双晶聚丁二酸丁二醇酯-聚丁二酸丁二醇酯(PES-b-PBS)多嵌段共聚物。用质子核磁共振波谱(1H核磁共振)对其组成和结构进行了表征。用标准差示扫描量热仪(DSC)、调温差示扫描量热仪(TMDSC)、偏光显微镜(POM)和广角X射线衍射仪(WAXD)研究了两块玻璃的非晶相相容性和晶化行为。当PbS和PES的嵌段长度小于4710gmol−1时，两块的无定形相是相容的。当嵌段长度增加到5430gmol−1以上时，两种嵌段的无定形相变为部分相容，并且随着嵌段长度的增加，相容程度降低。PBS和PES块体的结晶性能均随其块体尺寸的增大而增大。偏光显微镜观察表明，共聚物呈带状球晶形态，PBS嵌段结晶后，PES在有限的空间内结晶。WAXD分析表明，共聚物的结晶均由PES和PbS嵌段组成。
A series of biodegradable double crystalline poly(ethylene succinate)-b-poly(butylene succinate) (PES-b-PBS) multiblock copolymers with various PES and PBS block lengths were successfully synthesized by chain-extension reaction of dihydroxylated poly(ethylene succinate) (HO-PES-OH) and poly(butylene succinate) (HO-PBS-OH) using 1,6-hexamethylene diisocyanate (HDI) as a chain-extender. The compositions and structures were characterized by proton nuclear magnetic resonance spectroscopy (1H NMR). The miscibility of amorphous phase and crystallization behaviors of the two blocks were investigated by standard differential scanning calorimetry (DSC), temperature modulated DSC (TMDSC), polarized light optical microscopy (POM), and wide-angle X-ray diffraction (WAXD). When the block length of PBS and PES were less than 4710 g mol−1, the amorphous phases of the two blocks were miscible. As the block length increased to more than 5430 g mol−1, the amorphous phases of the two blocks changed to be partially miscible, and the miscibility decreased with further increasing the block lengths. The crystallizability of both PBS and PES blocks increased with an increase in size of their blocks. POM observation showed that the copolymers displayed banded spherulitic morphologies, and the crystallization of PES happened in confined space after crystallization of PBS blocks. WAXD analysis suggested that the crystals of the copolymers were composed of crystals of both PES and PBS blocks.