Comprehensive Characterization of Drying Oil Oxidation and Polymerization Using Time-Resolved Infrared Spectroscopy,Macromolecules

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Comprehensive Characterization of Drying Oil Oxidation and Polymerization Using Time-Resolved Infrared Spectroscopy
Macromolecules ( IF 5.1 ) Pub Date : 2024-08-27 , DOI: 10.1021/acs.macromol.4c01164
Gwen DePolo _{1,

2} , Piet Iedema ₂ , Kenneth Shull ₁ , Joen Hermans _{2,

3,

4}

Affiliation

Drying oils like linseed oil are composed of multifunctional triglyceride molecules that can cure through three-dimensional free-radical polymerization into complex polymer networks. In the context of oil paint conservation, it is important to understand how factors like paint composition and curing conditions affect the chemistry and network structure of the oil polymer network and subsequently the links between the structure and long-term paint stability. Here, we employed time-resolved ATR-FTIR spectroscopy and comprehensive data analysis to study the curing behavior of five types of drying oil and the effects of curing temperature as well as the presence of a curing catalyst (PbO). Extracted concentration curves of key reactive functional groups point to a phase transition similar to a gel point that is especially pronounced in the presence of PbO, after which curing reactivity slows down dramatically. Analysis of kinetic parameters suggests that PbO induces a network structure with a more heterogeneous cross-link density, and the ATR-FTIR spectra indicate lower levels of oxidation in those cases. Finally, lower temperatures appear to favor the formation of carboxylic acid groups in oil mixtures with PbO.

中文翻译：

使用时间分辨红外光谱全面表征干性油氧化和聚合

亚麻籽油等干性油由多功能甘油三酯分子组成，可以通过三维自由基聚合固化成复杂的聚合物网络。在油漆保护的背景下，了解油漆成分和固化条件等因素如何影响油聚合物网络的化学和网络结构以及随后的结构与长期油漆稳定性之间的联系非常重要。在这里，我们采用时间分辨 ATR-FTIR 光谱和综合数据分析来研究五种干性油的固化行为以及固化温度以及固化催化剂 (PbO) 的存在的影响。关键反应性官能团的提取浓度曲线表明，存在类似于凝胶点的相变，在 PbO 存在的情况下尤其明显，之后固化反应性急剧减慢。动力学参数分析表明，PbO 诱导出具有更异质交联密度的网络结构，并且 ATR-FTIR 光谱表明在这些情况下氧化水平较低。最后，较低的温度似乎有利于在含有 PbO 的油混合物中形成羧酸基团。

更新日期：2024-08-27

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