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S. Shyamroy B. Garnaik S. Sivaram 《Journal of polymer science. Part A, Polymer chemistry》2005,43(10):2164-2177
The synthesis of low‐molecular‐weight (weight‐average molecular weight < 45,000 g/mol) lactic acid polymers through the dehydropolycondensation of L ‐lactic acid was investigated. Polymerizations were carried out in solution with solvents (xylene, mesitylene, and decalin), without a solvent using different Lewis acid catalysts (tetraphenyl tin and tetra‐n‐butyldichlorodistannoxane), and at three different polymerization temperatures (143, 165, and 190 °C). The products were characterized with differential scanning calorimetry, size exclusion chromatography, vapor pressure osmometry, 13C NMR, and matrix‐assisted laser desorption/ionization time‐of‐flight (MALDI‐TOF). The resulting polymers contained less than 1 mol % lactide, as shown by NMR. The number‐average molecular weights were calculated from the ratio of the area peaks of ester carbonyl and carboxylic acid end groups via 13C NMR. The stereosequences were analyzed by 13C NMR spectroscopy on the basis of triad effects. Tetraphenyl tin was an effective transesterification catalyst, and the randomization of the stereosequence at 190 °C was observed. In contrast, the distannoxane catalyst caused comparatively less transesterification reaction, and the randomization of the stereosequences was slow even at 190 °C. The L ‐lactic acid and D ‐lactic acid isomers were added to the polymer chain in a small, blocky fashion. The MALDI‐TOF spectra of poly(L ‐lactic acid) (PLA) chains doped with Na+ and K+ cations showed that the PLA chains had the expected end groups. The MALDI‐TOF analysis also enabled the simultaneous detection of the cyclic oligomers of PLA present in these samples, and this led to the full structural characterization of the molecular species in PLA. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 2164–2177, 2005 相似文献
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通过调整溶液浓度和测试温度等测试参数,与文献[1]比较我们获得了无规聚丙烯腈(PAN)和部分全同PAN样品更高分辨率的13C核磁共振谱. 合理归属了次甲基碳的五单元组(mmmm、mmmr和rmmr)、腈基碳与次甲基碳的七单元组(mmmmmm、mmmmmr和rmmmmr)各特征峰. 无规PAN样品服从伯努利统计模型. 一级马尔科夫和二级马尔科夫统计模型分别被用于定量计算部分全同PAN样品的五单元组和七单元组的立构分布. 计算了不同立构规整度样品的“全同单元段”和“间同单元段”平均长度, 从另一方面证实了上述的七单元组归属的正确性. 相似文献
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