High-throughput microchannel flow technology for continuous nitration of benzene and chlorobenzene
苯和氯苯高通量微通道连续硝化技术探究
Zhang X. Wang M. Du B. Qu X. Li H. Yang L. An M. Yang Z. Moldyr D. Li W.
2025Tianjin University
Chemical Industry and Engineering
2025#42Issue 672 - 83 pp.
Aromatic nitration reaction poses challenges to the sustainable development of traditional batch synthesis process due to its rapid kinetics and significant exothermic nature. In contrast, microchannel flow technology offers crucial technical support for the safe, efficient, and environmentally friendly synthesis of such typical strong exothermic reactions. This work systematically investigated the control steps and process intensification strategies of high-throughput continuous nitration of benzene and chlorobenzene by utilizing annular tube-in-tube microchannel continuous flow technology. For the mononitration reaction, the conversion of benzene exceeds 99. 5%, yielding nitrobenzene (NB) at an impressive rate of 99% under the conditions comprising of mixed acid water content of 13%, nitric acid/benzene molar ratio of 1. 05 ∶1. 00, reaction temperature of 50 ℃ and residence time of 3 s. Similarly, chlorobenzene exhibits over 99. 5% conversion with a nitrochlorobenzene (NCB) yield reaching 99. 2% when subjects to a nitric acid/chlorobenzene molar ratio of 1. 2 ∶1. 0 at a reaction temperature of 40 ℃. For the dinitration reaction, under the conditions featuring a 3. 5% water content of mixed acid, a 90 ℃ reaction temperature and 156 s residence time, the total yield of dinitrobenzene (DNB) reaches up to 98. 5%, with m-isomers constituting 82. 5% thereof. At a nitric acid/chlorobenzene molar ratio of 2. 2 ∶1. 0, the yield of dinitrochlorobenzene (DNCB) is 98. 6% (2,4-DNCB accounted for > 95%). In the high-throughput (150 ~ 750 mL·min-1) scale-up process, the yields of mononitration products of benzene and chlorobenzene are 99. 3% and 99. 6%, respectively, and the yields of dinitration are 96. 4% and 96. 5%, respectively. Notably, no significant amplification effect was observed throughout these experiments.
benzene , chlorobenzene , high-throughput , microchannel flow , nitration reaction , process intensification
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School of Chemical Engineering and Technology, Zhengzhou University, Zhengzhou, 450001, China
Ningxia Tongde Love Cycle Energy Technology Co., Ltd., Ningxia, Wuzhong, 751305, China
School of Chemistry and Chemical Engineering, Shihezi University, Xinjiang, Shihezi, 832003, China
Faculty of Chemistry and Chemical Technology, Al-Farabi Kazakh National University, Almaty, 050051, Kazakhstan
School of Chemical Engineering and Technology
Ningxia Tongde Love Cycle Energy Technology Co.
School of Chemistry and Chemical Engineering
Faculty of Chemistry and Chemical Technology
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