In this study, kilogram-scale synthesis of 2-ethylhexyl nitrate in a microreactor was reported. Using Box–Behnken experimental design, the effects of process parameters such as temperature, molar ratio, total flow rate, and mass fraction of sulfuric acid on the yield of the target product were systematically investigated. The experimental design was studied at four factors and three levels. The results revealed that the sulfuric acid mass fraction and temperature significantly affected the yield of the product. There was a good agreement between the experimental results and predicted results by the proposed regression model. Subsequently, the mixing effect of the liquid–liquid heterogeneous system in microreactor was simulated by using computational fluid dynamics. The results provide solid evidence that the microreactor has excellent mixing efficiency in mass and heat transfer compared with the conventional reactor. Consequently, based on the results of process parameter optimization, an enlarged microreactor was designed to intensify the preparation of 2-ethylhexyl nitrate by a throughput of 16 kg/h.

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