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通过耦合时间分辨傅里叶变换红外光谱和重量测量研究甲醇/聚酰亚胺体系中的扩散和分子相互作用。

Diffusion and molecular interactions in a methanol/polyimide system probed by coupling time-resolved FTIR spectroscopy with gravimetric measurements.

机构信息

Institute of Chemistry and Technology of Polymers, National Research Council of Italy Naples, Italy.

Department of Chemical, Materials and Industrial Production Engineering, University of Naples Federico II Naples, Italy.

出版信息

Front Chem. 2014 Jan 30;2:2. doi: 10.3389/fchem.2014.00002. eCollection 2014.

DOI:10.3389/fchem.2014.00002
PMID:24809042
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC4010125/
Abstract

In this contribution the diffusion of methanol in a commercial polyimide (PMDA-ODA) is studied by coupling gravimetric measurements with in-situ, time-resolved FTIR spectroscopy. The spectroscopic data have been treated with two complementary techniques, i.e., difference spectroscopy (DS) and least-squares curve fitting (LSCF). These approaches provided information about the overall diffusivity, the nature of the molecular interactions among the system components and the dynamics of the various molecular species. Additional spectroscopic measurements on thin film samples (about 2 μm) allowed us to identify the interaction site on the polymer backbone and to propose likely structures for the H-bonding aggregates. Molar absorptivity values from a previous literature report allowed us to estimate the population of first-shell and second-shell layers of methanol in the polymer matrix. In terms of diffusion kinetics, the gravimetric and spectroscopic estimates of the diffusion coefficients were found to be in good agreement with each other and with previous literature reports. A Fickian behavior was observed throughout, with diffusivity values markedly affected by the total concentration of sorbed methanol.

摘要

本研究通过将重量法测量与原位、时间分辨傅里叶变换红外光谱法相结合，研究了甲醇在商业聚酰亚胺（PMDA-ODA）中的扩散。使用两种互补技术，即差谱法（DS）和最小二乘曲线拟合（LSCF）对光谱数据进行了处理。这些方法提供了有关整体扩散系数、系统成分之间分子相互作用的性质以及各种分子物种动力学的信息。对薄膜样品（约 2μm）的附加光谱测量使我们能够确定聚合物主链上的相互作用位点，并提出氢键聚集体的可能结构。从之前文献报告中的摩尔吸光率值，我们可以估计甲醇在聚合物基质中的第一壳层和第二壳层的浓度。在扩散动力学方面，重量法和光谱法估算的扩散系数彼此之间以及与之前的文献报告非常吻合。在整个过程中都观察到 Fickian 行为，扩散系数值明显受到吸附甲醇的总浓度的影响。

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本文引用的文献

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Combining gravimetric and vibrational spectroscopy measurements to quantify first- and second-shell hydration layers in polyimides with different molecular architectures.结合重量分析和振动光谱测量，定量分析具有不同分子结构的聚酰亚胺中的第一和第二壳层水合层。
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