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Process performance and kinetics of the esterification of diketene to methyl acetoacetate in helical continuous-flow microreactors
Chemical Engineering Science ( IF 4.7 ) Pub Date : 2022-08-04 , DOI: 10.1016/j.ces.2022.117970
Hui Zhou , Xian Tang , Zilai Wang , Yunhao Sun , Xiang Ling

The esterification of 4-methyleneoxetan-2-one (diketene) and methanol to obtain methyl acetoacetate (MAA) was conducted in a helical continuous-flow microreactor with triethylamine and 4-methylbenzenesulfonic acid (TsOH) as the catalyst in the absence of a solvent. The effects of the initial molar ratios of methanol to diketene and catalyst to diketene, reaction temperature, and residence time on the esterification reaction were also investigated and optimized. Under optimal conditions, the yield and selectivity of the reaction system for MAA exceeded 97% with only 120 s. In addition, a kinetic model of the esterification reaction inside helical continuous-flow microreactor was established with acceptable model performance. This work demonstrates that the combination of helical continuous flow and esterification, which is designed to provide researchers with a unique process, is also key to assessing the relevant esterification mechanism.



中文翻译:

双烯酮酯化成乙酰乙酸甲酯在螺旋连续流动微反应器中的工艺性能和动力学

以三乙胺和4-甲基苯磺酸(TsOH)为催化剂,在无溶剂条件下,4-亚甲基氧杂环丁烷-2-酮(双烯酮)与甲醇酯化得到乙酰乙酸甲酯(MAA)。 . 还研究和优化了甲醇与双烯酮和催化剂与双烯酮的初始摩尔比、反应温度和停留时间对酯化反应的影响。在最佳条件下,MAA反应体系的产率和选择性均在120 s内超过97%。此外,建立了螺旋连续流动微反应器内酯化反应的动力学模型,模型性能可接受。这项工作证明了螺旋连续流动和酯化的结合,

更新日期:2022-08-04
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