Crystalline/amorphous phase structure and molecular mobility of biodegradable poly(butylene adipate-co-butylene terephthalate) and related polyesters.
Crystalline/amorphous phase structure and molecular mobility of biodegradable poly(butylene adipate-co-butylene terephthalate) and related polyesters.
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DOI：
10.1021/bm0156476
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发表时间：
2002-01
影响因子：
6.2
通讯作者：
K. Kuwabara;Z. Gan;Takashi Nakamura;H. Abe;Y. Doi
中科院分区：
文献类型：
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作者：
K. Kuwabara;Z. Gan;Takashi Nakamura;H. Abe;Y. Doi
采用差示扫描量热法（DSC）、原子力显微镜（AFM）、广角x射线散射（WAXD）和固态（13）C NMR研究了熔融结晶的可生物降解聚（己二酸丁二酯-co-44 mol %对苯二甲酸丁二酯）[P(BA-co-44 mol % BT)]共聚酯样品的结晶/非晶结构和分子迁移率。DSC吸热峰，这是归因于晶体区域的融化，是广泛的相对于常规部分结晶聚酯的报道。在AFM观察中，未观察到球晶形态，仅检测到100 nm左右的小颗粒。样品的WAXD模式非常宽。这些结果表明，熔融结晶的P（BA-co-44 mol % BT）样品含有小晶体，尺寸分布广泛。固态（13）C核磁共振技术也被用于对对苯二甲酸丁二酯和己二酸丁二酯单位进行分子水平和选择性分析。对于对苯二甲酸丁二酯单元，检测到两种具有不同微观结构和分子迁移率的组分的存在：一种组分被分配到聚对苯二甲酸丁二酯均聚物（PBT）的α型晶体中，另一种组分在无定形区域中。相反，所有的己二酸丁烯单元都位于无定形区域。固体核磁共振数据表明，晶体区域的尺寸小于3nm。
Differential scanning calorimetry (DSC), atomic force microscopy (AFM), wide-angle X-ray scattering (WAXD), and solid-state (13)C NMR have been used to investigate the crystalline/amorphous structure and molecular mobility of biodegradable poly(butylene adipate-co-44 mol % butylene terephthalate) [P(BA-co-44 mol % BT)] copolyester sample crystallized from the melt. The DSC endothermic peak, which is ascribed to the melting of the crystalline region, was broad relative to those reported for conventional partially crystalline polyesters. In AFM observation, spherulitic morphology was not observed while small particles with a size of about 100 nm were detected. The WAXD pattern of the sample was very broad. These results have indicated that a melt-crystallized P(BA-co-44 mol % BT) sample contains small crystals with a wide distribution in size. A solid-state (13)C NMR technique was also used to perform molecular-level and selective analyses for both butylene terephthalate and butylene adipate units. For the butylene terephthalate units, the existence of two components with different microstructure and molecular mobility was detected: one component was assigned to the alpha-form crystal of poly(butylene terephthalate) homopolymer (PBT) and the other was in amorphous regions. In contrast, all of butylene adipate units were located in amorphous regions. Solid-state NMR data have suggested that sizes of crystalline regions are less than 3 nm.