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Use of Dielectric Spectroscopy for Real-Time In-situ Reaction Monitoring

机译:介电谱用于实时原位反应监测

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Coating resin manufacturing requires knowledge of the extent of reaction during resin synthesis so the appropriate actions can be taken (addition of the next reactant,reaction termination,etc.).This article reports the results from experiments conducted to survey the utility of dielectric spectroscopy (DES) as a real-time,in-situ technique to monitor the extent of reaction during synthesis of three low molecular weight resins that are representative of components used in coatings formulations.The resins made were based on very different chemistries:(1) a 100% solids polyacrylate functional oligomer from the Michael reaction between a polyacrylate monomer and an acetoacetate ester;(2) an acrylate functional monomer from the reaction between an epoxy ester and acrylic acid;and (3) a solvent-based isocyanate-ter-minated polyurethane prepolymer from the reaction between a mixture of diols and excess diisocyanate.In all three cases,very good to excellent correlations were found between continuous real-time DES output and the values of characteristic QC parameters (viscosity,acid number,epoxy equivalent weight,% NCO,ATR-FTIR peak heights for reactants and products,and GPC data) determined by off-line analysis of samples taken periodically during the reactions.
机译:涂料树脂的生产需要了解树脂合成过程中的反应程度,因此可以采取适当的措施(添加下一个反应物,终止反应等)。本文报道了为调查介电光谱的效用而进行的实验结果( DES)是一种实时的原位技术,用于监控三种低分子量树脂在合成过程中的反应程度,这些低分子量树脂代表了涂料配方中使用的组分。制备的树脂基于非常不同的化学性质:(1)a来自聚丙烯酸酯单体与乙酰乙酸酯之间的迈克尔反应的100%固体聚丙烯酸酯官能低聚物;(2)来自环氧酯与丙烯酸之间反应的丙烯酸酯官能单体;和(3)溶剂基异氰酸酯末端封端二醇和过量的二异氰酸酯之间的反应生成的聚氨酯预聚物。在所有三种情况下,cont之间的相关性都非常好。通过定期对样品进行离线分析确定的非连续实时DES输出和特征性QC参数值(粘度,酸值,环氧当量,%NCO,ATR-FTIR反应物和产物的峰高以及GPC数据)在反应期间。

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