Chen Miao, Zhang Guangxu, Wang Ruolin
School of Chemistry, Chemical Engineering and Life Sciences, Wuhan University of Technology, Wuhan 430070, China.
Materials (Basel). 2025 Mar 17;18(6):1315. doi: 10.3390/ma18061315.
Polybutylene succinate (PBS) is a biodegradable aliphatic polyester with excellent thermal stability, mechanical properties, and processability. The synthesis of PBS typically employs titanium-based catalysts like tetrabutyl titanate (TBT) to accelerate the reaction. However, TBT acts as a homogeneous catalyst and is non-recyclable. This study aims to minimize the cost of recovering liquid TBT catalyst during PBS synthesis by using TBT-loaded activated carbon for direct esterification and optimizing the process conditions. The catalyst was analyzed using inductively coupled plasma emission spectroscopy, automated specific surface area and pore size analysis, X-ray diffraction, and Fourier-transform infrared spectroscopy. The product was evaluated through infrared spectroscopy, nuclear magnetic resonance hydrogen spectra, and gel permeation chromatography. The optimal process parameters were determined to be an esterification temperature of 170 °C, a polycondensation temperature of 235 °C, an acid-to-alcohol molar ratio of 1:1.2, a catalyst amount of 0.06 g, and a dehydration time of 3 h. Under these conditions, the weight-average molecular weight of PBS reached 47,655, reducing the catalyst usage from 0.5% to 0.3%, resulting in a 24.7% increase in catalytic efficiency compared to TBT, significantly lowering costs. After five cycles of reuse, the weight-average molecular weight of the product remained above 35,000. This study demonstrates that TBT-loaded activated carbon exhibits superior catalytic performance, offering a cost-effective and efficient method for industrial PBS production with broad application potential.
聚丁二酸丁二醇酯（PBS）是一种可生物降解的脂肪族聚酯，具有优异的热稳定性、机械性能和加工性能。PBS的合成通常采用钛基催化剂，如钛酸四丁酯（TBT）来加速反应。然而，TBT作为均相催化剂，不可回收。本研究旨在通过使用负载TBT的活性炭进行直接酯化并优化工艺条件，将PBS合成过程中回收液态TBT催化剂的成本降至最低。采用电感耦合等离子体发射光谱、自动比表面积和孔径分析、X射线衍射和傅里叶变换红外光谱对催化剂进行了分析。通过红外光谱、核磁共振氢谱和凝胶渗透色谱对产物进行了评估。确定最佳工艺参数为酯化温度170℃、缩聚温度235℃、酸醇摩尔比1:1.2、催化剂用量0.06 g、脱水时间3 h。在此条件下，PBS的重均分子量达到47655，催化剂用量从0.5%降至0.3%，与TBT相比催化效率提高了24.7%，显著降低了成本。经过五次重复使用循环后，产物的重均分子量仍保持在35000以上。本研究表明，负载TBT的活性炭具有优异的催化性能，为工业PBS生产提供了一种经济高效的方法，具有广阔的应用潜力。
