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基于异山梨醇的生物基热塑性聚缩醛一步法优化合成

Optimized Synthesis According to One-Step Process of a Biobased Thermoplastic Polyacetal Derived from Isosorbide.

作者信息

Hammami Nadia, Jarroux Nathalie, Robitzer Mike, Majdoub Mustapha, Habas Jean-Pierre

机构信息

Institut Charles Gerhardt, CC 1702, Place E. Bataillon, 34095 Montpellier, France.

Laboratoire des Interfaces et Matériaux Avancés, Université de Monastir, 5000 Monastir, Tunisia.

出版信息

Polymers (Basel). 2016 Aug 10;8(8):294. doi: 10.3390/polym8080294.

DOI:10.3390/polym8080294
PMID:30974571
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6431881/
Abstract

This paper describes both the synthesis and characterization of a biobased and non-aromatic polyacetal produced from the reaction between isosorbide and methylene chloride. The reaction was conducted in an aprotic dipolar and harmless solvent using a one-step, fast and economical procedure. The chemical composition of this polymer was investigated using Nuclear Magnetic Resonance and Fourier Transform Infra-Red spectroscopies. The molecular weights were examined by size exclusion chromatography and MALDI-TOF spectrometry. The synthesis conditions (concentration, mixing speed, solvent nature, stoichiometry, addition mode of one reactan) were found to strongly influence both polymer architecture and reaction yield. Under moderated stirring conditions, the polyacetal was characterized by a larger amount of macro-cycles. Inversely, under higher intensity mixing and with an excess of methylene chloride, it was mainly composed of linear chains. In this latter case, the polymeric material presented an amorphous morphology with a glass transition temperature () close to 55 °C. Its degradation temperature was evaluated to be close to 215 °C using thermogravimetry according to multi-ramp methodology. The chemical approach and the physicochemical properties are valuable in comparison with that characteristic of other isosorbide-based polyacetals.

摘要

本文描述了由异山梨醇与二氯甲烷反应制得的一种生物基非芳香族聚缩醛的合成及表征。该反应在非质子偶极且无害的溶剂中采用一步法、快速且经济的程序进行。使用核磁共振和傅里叶变换红外光谱对该聚合物的化学组成进行了研究。通过尺寸排阻色谱法和基质辅助激光解吸电离飞行时间质谱法对分子量进行了检测。发现合成条件（浓度、混合速度、溶剂性质、化学计量比、一种反应物的添加方式）对聚合物结构和反应产率均有强烈影响。在适度搅拌条件下，聚缩醛的特征是含有大量大环结构。相反，在更高强度混合且二氯甲烷过量的情况下，它主要由线性链组成。在后一种情况下，该聚合物材料呈现无定形态，玻璃化转变温度接近55℃。根据多升温速率方法，使用热重分析法评估其降解温度接近215℃。与其他基于异山梨醇的聚缩醛的特性相比，这种化学方法和物理化学性质具有重要价值。

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