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聚（L-丙交酯-己二酸丁二酯-L-丙交酯）三嵌段共聚物中聚己二酸丁二酯中间嵌段的多晶型结晶行为

Polymorphic Crystallization Behavior of a Poly(butylene adipate) Midblock within a Poly(L-lactide-butylene adipate-L-lactide) Triblock Copolymer.

作者信息

Hua Lei, Wang Xiaodong

机构信息

Institute of Polymer Science and Engineering, TongJi Zhejiang College, Jiaxing 314051, China.

Jiaxing Key Laboratory of High-Performance and Functional Materials in Civil and Environmental Engineering, Tongji Zhejiang College, Jiaxing 314051, China.

出版信息

Polymers (Basel). 2022 Nov 13;14(22):4902. doi: 10.3390/polym14224902.

DOI:10.3390/polym14224902
PMID:36433028
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9696281/
Abstract

New biodegradable aliphatic PLLA-PBA-PLLA copolymers with soft poly(butylene adipate) (PBA) and hard poly(l-lactide) (PLLA) building blocks were synthesized via ring-opening polymerization (ROP). Proton nuclear magnetic resonance (HNMR) was utilized to confirm the volume fraction of PBA (f) within PLLA-PBA-PLLA. It was found that a PBA midblock (PBA-mid) within PLLA-PBA-PLLA-s (PLLA-PBA-PLLA triblock copolymer with a short PLLA block length) might display lamellar domain structure. However, PBA-mid within PLLA-PBA-PLLA-l (PLLA-PBA-PLLA triblock copolymer with a long PLLA block length) might locate itself as a nanoscale cylindrical domain surrounded by a PLLA continuous phase. Polymorphic crystals of PBA-mid within the PLLA-PBA-PLLA copolymers were formed after melt crystallization at the given temperatures, which were studied by differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD) analysis. According to the WAXD and DSC analyses, it was interesting to find that the α-type crystal of PBA-mid was favorable to develop in the lower temperature region regardless of the state (crystallization or amorphous) of the PLLA component. Additionally, when the PLLA component was held in its amorphous state, it was easier for PBA-mid within the PLLA-PBA-PLLA copolymers to transform from the metastable β-form crystal to the stable α-form crystal. Furthermore, polarized optical microscopy (POM) photos provided direct evidence of the polymorphic crystals of PBA-mid within PLLA-PBA-PLLAs.

摘要

通过开环聚合（ROP）合成了具有软质聚（己二酸丁二醇酯）（PBA）和硬质聚（L-丙交酯）（PLLA）结构单元的新型可生物降解脂肪族PLLA-PBA-PLLA共聚物。利用质子核磁共振（HNMR）来确定PLLA-PBA-PLLA中PBA的体积分数（f）。研究发现，PLLA-PBA-PLLA-s（PLLA嵌段长度较短的PLLA-PBA-PLLA三嵌段共聚物）中的PBA中间嵌段（PBA-mid）可能呈现层状畴结构。然而，PLLA-PBA-PLLA-l（PLLA嵌段长度较长的PLLA-PBA-PLLA三嵌段共聚物）中的PBA-mid可能以纳米级圆柱状畴的形式存在，周围是PLLA连续相。在给定温度下熔融结晶后，PLLA-PBA-PLLA共聚物中的PBA-mid形成了多晶型晶体，通过差示扫描量热法（DSC）和广角X射线衍射（WAXD）分析对其进行了研究。根据WAXD和DSC分析，有趣的是发现无论PLLA组分的状态（结晶或非晶）如何，PBA-mid的α型晶体在较低温度区域更易于形成。此外，当PLLA组分保持在非晶态时，PLLA-PBA-PLLA共聚物中的PBA-mid更容易从亚稳的β型晶体转变为稳定的α型晶体。此外，偏光显微镜（POM）照片提供了PLLA-PBA-PLLAs中PBA-mid多晶型晶体的直接证据。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/b8948390e3ce/polymers-14-04902-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/ce812f0e252d/polymers-14-04902-g001.jpg
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https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/30f2fb7c24ff/polymers-14-04902-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/719b0f7c295c/polymers-14-04902-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/f46730ce51ab/polymers-14-04902-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/75f0ba155411/polymers-14-04902-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/5c78218bc1a6/polymers-14-04902-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/4d78d6352041/polymers-14-04902-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/827dde8567ed/polymers-14-04902-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/b8948390e3ce/polymers-14-04902-g011.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/ce812f0e252d/polymers-14-04902-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/97e20f812d9e/polymers-14-04902-g002a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/347fa95d22e7/polymers-14-04902-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/30f2fb7c24ff/polymers-14-04902-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/719b0f7c295c/polymers-14-04902-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/f46730ce51ab/polymers-14-04902-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/75f0ba155411/polymers-14-04902-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/5c78218bc1a6/polymers-14-04902-g008.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/4d78d6352041/polymers-14-04902-g009.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/827dde8567ed/polymers-14-04902-g010.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/238f/9696281/b8948390e3ce/polymers-14-04902-g011.jpg

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本文引用的文献

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Polysaccharide-based nanofibers for pharmaceutical and biomedical applications: A review.多糖基纳米纤维在药物和生物医学中的应用：综述。
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Melt crystallization and crystal transition of poly(butylene adipate) revealed by infrared spectroscopy.红外光谱揭示聚己二酸丁二醇酯的熔融结晶与晶体转变
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Metastability and transformation of polymorphic crystals in biodegradable poly(butylene adipate).可生物降解聚己二酸丁二醇酯中多晶型晶体的亚稳态与转变
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Syntheses and physical characterization of new aliphatic triblock poly(L-lactide-b-butylene succinate-b-L-lactide)s bearing soft and hard biodegradable building blocks.新型含软质和硬质可生物降解结构单元的脂肪族三嵌段聚（L-丙交酯-b-丁二酸丁二酯-b-L-丙交酯）的合成与物理表征
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