新戊二醇与乙酸和 2-乙基己酸发生酯化反应的动力学规律

D. S. Chicheva, E. L. Krasnykh, V. A. Shakun
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摘要

目标。开发一种以氧化合成产物新戊二醇(NPG)为基础生产环保型非邻苯二甲酸酯增塑剂、润滑剂和变压器油的国内技术。研究方法是在单羧酸摩尔过量 8 倍的自催化条件下,研究 NPG 与乙酸和 2-乙基己酸酯化的动力学规律。在溶剂苯和间二甲苯的存在下,通过共沸酯化反应生成 NPG 酯。所得二酯通过真空整流从反应物中分离出来。所得 NPG 二酯的纯度不低于 99.7 wt %。采用红外光谱法、气相色谱-质谱法和气液相色谱法对反应样品进行了定性和定量成分分析。本文介绍了 NPG 与乙酸和 2- 乙基己酸酯化反应的动力学研究结果。它比较了所用酸的反应速率和反应活性。在给定的条件下,生成了 NPG 二酯,并测定了它们的一些理化性质。这使得所获得的数据可用于开发生产 NPG 二酯的工业技术。研究表明,在自催化条件下,酸摩尔过量为 8 倍时,最佳工艺温度为 100-110℃ ,20-22 小时内可获得 95% 的 NPG 二乙酸酯产率;最佳工艺温度为 160-170℃ ,26-28 小时内可获得 NPG 二(2-乙基己酸)酯产率。建立了 NPG 与乙酸和 2-乙基己酸形成单酯和二酯的活化能和预指数。论文介绍了酯化的动力学模型。
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Kinetic regularities of neopentyl glycol esterification with acetic and 2-ethylhexanoic acids
Objectives. Development of a domestic technology for producing environmentally friendly non-phthalate plasticizers, lubricants and transformer fluids based on neopentyl glycol (NPG), an oxo-synthesis product.Methods. The methodology of the work was to study the kinetic laws of NPG esterification with acetic and 2-ethylhexanoic acids under self-catalysis conditions with an 8-fold molar excess of monocarboxylic acids. The production of NPG esters was carried out by azeotropic esterification in the presence of solvents—benzene and m-xylene. The resulting diesters were isolated from the reaction mass by vacuum rectification. The purity of the obtained NPG diesters was no less than 99.7 wt %. Analysis of the qualitative and quantitative composition of reaction samples was carried out using infrared spectroscopy, gas chromatography–mass spectrometry and gas–liquid chromatography.Results. The paper presents the results of kinetic studies on NPG esterification of with acetic and 2-ethylhexanoic acids. It compares the reaction rates and reactivity of the acids used. Under the given conditions, NPG diesters were produced, and some of their physicochemical properties were determined. This enabled the data obtained to be used for the development of industrial technology in the production of NPG diesters.Conclusions. It was established that with an eightfold molar excess of acid under self-catalysis conditions, a yield of NPG diacetate equal to 95% is achieved within 20–22 h at an optimal process temperature of 100–110℃; NPG di(2-ethylhexanoate)—within 26–28 h at 160–170℃. The activation energies and pre-exponential factors for the formation of NPG mono- and diesters with acetic and 2-ethylhexanoic acids were established. The paper presents the kinetic models of esterification.
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