聚丁二酸丁二醇酯环状二聚物的纯化、表征及其开环聚合的研究

从聚丁二酸丁二醇酯(PBS)的环状低聚物中分离提纯出了PBS的环状二聚物〔cyclic dimer of poly(butylenesuccinate),CDBS〕,采用核磁、质谱对该环状二聚物进行了表征,研究表明,通过分离纯化得到了纯度高的PBS的环状二聚物。以纯化的CDBS为原料、十二醇为初始剂、辛酸锡作催化剂,采用开环聚合的方法合成了PBS,采用核磁、红外光谱对合成的PBS的结构进行了表征,并研究了开环聚合温度、聚合时间以及催化剂用量对PBS的分子量、单体转化率的影响,结果表明,开环反应温度220℃左右,反应3 h,PBS的相对分子质量(简称分子量,下同)可达到63 300,与直接酯化-缩聚法相比,采用开环聚合法能提高PBS的制备效率。

Purification, characterization and ring-opening polymerization of cyclic dimer of butylenes succinate

Cyclic dimer of butylene succinate (CDBS) was purified from the crude cyclic oligomers of butylene succinate. The purified CDBS was characterized by 1H NMR spectrum and mass spectra. The purified CDBS was subjected to ring-opening polymerization (ROP) to obtain poly(butylene succinate) (PBS) with 1-dodecanol as the initiator and tin octoate as the catalyst. The resultant PBS was characterized by Fourier transform infrared (FTIR) spectroscopy and 1H NMR spectrum. The effect of ROP temperature, ROP time and catalyst content on molecular weight of PBS and conversion were also investigated. The results show that, ROP can obtain the high-molecular-weight PBS, the highest number-average molecular weight (Mn) reached about 63.3 kDa in 3 h at 220 °C.