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傅里叶变换红外光谱结合振荡流变学:如何评估含马来酸酐相容剂酯衍生物的化学结构。

FT-IR combined with oscillatory rheology: How to evaluate chemical structure of ester derivatives of MA-containing compatibilizers.

作者信息

Varga Csilla, Simon-Stőger Lilla

机构信息

Sustainability Solutions Research Lab, University of Pannonia, 10. Egyetem Str., Veszprém, 8200, Hungary.

出版信息

Heliyon. 2024 Mar 30;10(7):e28948. doi: 10.1016/j.heliyon.2024.e28948. eCollection 2024 Apr 15.

DOI:10.1016/j.heliyon.2024.e28948
PMID:38601537
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11004813/
Abstract

Ester derivatives of experimental olefin-maleic anhydride copolymers synthesized at the University of Pannonia have been investigated by both classical and instrumental analytical methods that contribute to a deeper understanding of how that type of additives functions as compatibilizers for plastics and rubbers. Titration-based acid and saponification numbers have provided limited information about the chemical structure of the experimental copolymer compounds. A prompt, precise and low-cost method or combination of methods has been required to access to the ratio of the various derivatives not only straight after esterification but also for quality control during long-term storage considering the even stricter sustainability aspects either. Reproduction and scaling-up synthesises can be also followed by the combined measuring techniques of Fourier-transform infrared spectroscopy (FT-IR) and oscillatory rheometry. Structural changes occurred in the additives could be followed through monitoring their Ester Indices (EI) during the measurement, which can be connected also to the long-term properties. Experimental additives (AD) like AD-1 and AD-2 types with lower EI values of 21.5 % and 32.1 %, respectively, resulted in higher upper limits of the linear viscoelastic (LVE) range (15 % and 10 %). Conversely, the higher EI values of AD-3 and AD-4 led to significantly lower or even immeasurable upper limits of the LVE range. Additives with solid behaviour showed slight dependence on frequency above the crossover point that indicated strong connections disappearing.

摘要

潘诺尼亚大学合成的实验性烯烃 - 马来酸酐共聚物的酯衍生物已通过经典分析方法和仪器分析方法进行了研究,这些方法有助于更深入地了解这类添加剂如何作为塑料和橡胶的增容剂发挥作用。基于滴定的酸值和皂化值提供了关于实验共聚物化合物化学结构的有限信息。需要一种快速、精确且低成本的方法或方法组合,不仅要在酯化后直接获取各种衍生物的比例,还要考虑到更严格的可持续性方面,在长期储存期间进行质量控制。傅里叶变换红外光谱(FT - IR)和振荡流变学的联合测量技术也可用于跟踪复制和放大合成过程。在测量过程中,可以通过监测添加剂的酯指数(EI)来跟踪添加剂中发生的结构变化,这也可以与长期性能相关联。实验添加剂(AD)如AD - 1和AD - 2类型,其EI值分别较低,为21.5%和32.1%,导致线性粘弹性(LVE)范围的上限较高(分别为15%和10%)。相反,AD - 3和AD - 4的较高EI值导致LVE范围的上限显著降低甚至无法测量。具有固体行为的添加剂在交叉点以上对频率表现出轻微的依赖性,这表明强连接消失。

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本文引用的文献

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Effect of silane coupling agent on compatibility interface and properties of wheat straw/polylactic acid composites.硅烷偶联剂对麦秸/聚乳酸复合材料相容性界面及性能的影响。
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Catalyst-free esterification of high amylose starch with maleic anhydride in 1-butyl-3-methylimidazolium chloride: The effect of amylose content on the degree of MA substitution.无催化剂条件下 1-丁基-3-甲基咪唑氯盐中高直链淀粉与马来酸酐的酯化反应:直链淀粉含量对 MA 取代度的影响。
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Chemical Modification of Butyl Rubber with Maleic Anhydride via Nitroxide Chemistry and Its Application in Polymer Blends.
通过氮氧自由基化学对丁基橡胶进行马来酸酐化学改性及其在聚合物共混物中的应用
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A simple and convenient method for the hydrolysis of styrene-maleic anhydride copolymers to styrene-maleic acid copolymers.一种简单方便的水解苯乙烯-马来酸酐共聚物为苯乙烯-马来酸共聚物的方法。
Chem Phys Lipids. 2019 Jan;218:85-90. doi: 10.1016/j.chemphyslip.2018.11.011. Epub 2018 Dec 1.
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Olefin-maleic-anhydride copolymer based additives: a novel approach for compatibilizing blends of waste polyethylene and crumb rubber.基于烯烃-马来酸酐共聚物的添加剂:一种使废聚乙烯与胶粉共混物增容的新方法。
Waste Manag. 2015 Apr;38:65-71. doi: 10.1016/j.wasman.2015.01.004. Epub 2015 Jan 30.