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首页> 外文期刊>Journal of Applied Polymer Science >Solid state polymerization in a micro-reactor: The case of poly(tetramethylene terephthalamide)
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Solid state polymerization in a micro-reactor: The case of poly(tetramethylene terephthalamide)

机译：微反应器中的固态聚合：聚对苯二甲酸丁二醇酯

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The aim of this work was to develop and optimize a direct solid state polymerization (DSSP) process on a micro scale for alkyldiammonium-terephthalate salts. This was successfully demonstrated for the first time by the case of tetramethylenediammonium-terepththalate salt (4T salt). The derived polymer (PA4T) presents interesting properties, but the temperature-favored acid catalyzed cyclization of tetramethylenediamine (TMD) to mono-functional pyrrolidine and ammonia inhibits a high polymerization conversion. DSSP was performed in a thermogravimetrical analysis (TGA) chamber, and the continuously monitored weight loss was correlated to polymerization conversion via the release of water, excluding any mass and heat transfer limitations. It was found that the conditions under which the DSSP is performed and the morphology of the starting material affect both the reaction rate and the product quality. The effect of the critical process parameters, namely vent size, heating rate to reach SSP temperature, and reaction temperature were quantified by the observed mass loss and by H-1 NMR analysis. It was noticed that, besides the water formed by amidation, other volatile compounds were also released during the DSSP reaction, with main component, the TMD. In particular, it was observed that conditions favoring the evaporation of TMD also favored a higher reaction rate. The TMD loss was minimized by optimization of the aforementioned process conditions, leading to a more thermally stable and a higher molecular weight final product. The thermal stability of the PA4T was found to be inversely correlated to the concentration of carboxylic end groups present in the formed polymer. (c) 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 43271.
机译：这项工作的目的是在微观规模上开发和优化烷基对苯二甲酸二苯二铵盐的直接固态聚合（DSSP）工艺。四亚甲基二铵-对苯二甲酸乙酯盐（4T盐）首次成功地证明了这一点。衍生的聚合物（PA4T）表现出令人感兴趣的性能，但是温度促进酸催化的四亚甲基二胺（TMD）环化为单官能吡咯烷和氨会抑制高聚合转化率。 DSSP在热重分析（TGA）室中进行，连续监测的重量损失与水的释放与聚合转化率相关，不包括质量和传热限制。发现进行DSSP的条件和原料的形态影响反应速率和产物质量。通过观察到的质量损失和H-1 NMR分析，可以量化关键工艺参数（即排气口尺寸，达到​​SSP温度的加热速率和反应温度）的影响。注意到，除了由酰胺化形成的水以外，在DSSP反应期间还释放了其他挥发性化合物，其主要成分为TMD。特别地，观察到有利于TMD蒸发的条件也有利于更高的反应速率。通过优化上述工艺条件，可将TMD损失降至最低，从而获得更高的热稳定性和更高的分子量。发现PA4T的热稳定性与形成的聚合物中存在的羧基端基的浓度成反比。 （c）2015 Wiley Periodicals，Inc. J. Appl。 Polym。科学2016，133，43271。

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