Department of Polymer Chemistry, Zernike Institute for Advanced Materials, University of Groningen, Nijenborgh 4, 9747 AG Groningen, The Netherlands.
Biomolecules. 2013 Aug 12;3(3):461-80. doi: 10.3390/biom3030461.
Bio-based commercially available succinate, itaconate and 1,4-butanediol are enzymatically co-polymerized in solution via a two-stage method, using Candida antarctica Lipase B (CALB, in immobilized form as Novozyme® 435) as the biocatalyst. The chemical structures of the obtained products, poly(butylene succinate) (PBS) and poly(butylene succinate-co-itaconate) (PBSI), are confirmed by 1H- and 13C-NMR. The effects of the reaction conditions on the CALB-catalyzed synthesis of PBSI are fully investigated, and the optimal polymerization conditions are obtained. With the established method, PBSI with tunable compositions and satisfying reaction yields is produced. The 1H-NMR results confirm that carbon-carbon double bonds are well preserved in PBSI. The differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) results indicate that the amount of itaconate in the co-polyesters has no obvious effects on the glass-transition temperature and the thermal stability of PBS and PBSI, but has significant effects on the melting temperature.
通过两步法在溶液中将市售的生物基琥珀酸、衣康酸和 1,4-丁二醇用 Candida antarctica Lipase B（CALB，以固定化形式 Novozyme® 435 存在）作为生物催化剂进行酶法共聚。通过 1H-NMR 和 13C-NMR 确认了所得产物聚丁二酸丁二醇酯（PBS）和聚丁二酸丁二醇酯-共衣康酸酯（PBSI）的化学结构。全面研究了反应条件对 CALB 催化合成 PBSI 的影响，并获得了最佳聚合条件。采用所建立的方法，可以制备出具有可调组成和令人满意的反应收率的 PBSI。1H-NMR 结果证实 PBSI 中很好地保留了碳-碳双键。差示扫描量热法（DSC）和热重分析（TGA）结果表明，共聚酯中衣康酸的含量对 PBS 和 PBSI 的玻璃化转变温度和热稳定性没有明显影响，但对其熔融温度有显著影响。
