Synthesis and Characterization of Diethyl Citrate and Phase Equilibria in Mixtures with Ethanol and Water,Journal of Chemical & Engineering Data

当前位置： X-MOL 学术 › J. Chem. Eng. Data › 论文详情

Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)

Synthesis and Characterization of Diethyl Citrate and Phase Equilibria in Mixtures with Ethanol and Water
Journal of Chemical & Engineering Data ( IF 2.0 ) Pub Date : 2018-06-06 , DOI: 10.1021/acs.jced.7b01060
Claudia E. Berdugo ₁ , Andrea Suaza ₁ , Miguel A. Santaella ₁ , Orlando A. Sánchez ₁ , Gerardo Rodríguez ₁ , Alvaro Orjuela ₁

Affiliation

In this work, diethyl citrate (DEC) was synthesized and isolated for further physicochemical characterization and phase equilibria study. The synthesis was performed via partial esterification of citric acid with ethanol, and the final product was separated from the resulting mixture using a pH-controlled solvent extraction method. Characterization using ¹H NMR and ¹³C NMR spectroscopy confirmed the presence of both DEC isomers with few impurities. Results indicate that a 6:5 molar ratio of the symmetric to the nonsymmetric ester structures was attained during synthesis. Thermogravimetric analysis and differential scanning calorimetry allowed us to measure, for the first time, glass transition temperature (228 K) and decomposition temperature (493 K) of diethyl citrate. Additionally, P–x data for the vapor–liquid equilibrium of the binary mixtures diethyl citrate + ethanol and diethyl citrate + water were collected at 308 K using an accurate dynamic device. Data were regressed to generate binary interaction parameters for the UNIQUAC equation. The regressed model shows good agreement with experiments, and it can be used for further process design in the esterification of citric acid.

中文翻译：

乙醇和水混合物中柠檬酸二乙酯的合成，表征和相平衡

在这项工作中，柠檬酸二乙酯（DEC）进行了合成和分离，以用于进一步的物理化学表征和相平衡研究。通过柠檬酸与乙醇的部分酯化进行合成，并使用pH控制的溶剂萃取方法从所得混合物中分离出最终产物。使用¹ H NMR和¹³ C NMR光谱进行的表征证实了几乎没有杂质的两种DEC异构体均存在。结果表明，在合成过程中，对称与非对称酯结构的摩尔比为6：5。热重分析和差示扫描量热法使我们首次能够测量柠檬酸二乙酯的玻璃化转变温度（228 K）和分解温度（493 K）。此外，使用精确的动态装置在308 K下收集了柠檬酸二乙酯+乙醇和柠檬酸二乙酯+水的二元混合物的气液平衡的Px数据。对数据进行回归以生成UNIQUAC方程的二元相互作用参数。回归模型与实验结果吻合良好，可用于柠檬酸酯化的进一步工艺设计。

更新日期：2018-06-07

点击分享查看原文

点击收藏

阅读更多本刊最新论文