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Continuous and Safe Alkylation of 1,3,5-Trihydroxy-2,4,6-trinitrobenzene using Wiped Film Evaporator/Distillation Coupled Technology
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2022-08-22 , DOI: 10.1021/acs.oprd.2c00105
Xingyu Shao 1 , Wei Feng 2 , Zichao Guo 1 , Wanghua Chen 1
Affiliation  

Alkylation of 1,3,5-trihydroxy-2,4,6-trinitrobenzene (TNPG) is a key reaction to the synthesis of 2,4,6-trinitrobenzene-1,3,5-triamine, which is a famous insensitive high-energy material. Running this alkylation in the traditional stirred reactors has a high risk of spill and eruption incidents because of the evaporation of large amounts of volatile side-products. In this work, a wiped film evaporator/distillation coupled technology was used to run this reaction in a continuous and safe way. The design of the operation parameters was based on thorough understandings on reaction kinetics, residence time distribution, and heat transfer capacity of the wiped film evaporator. The results showed that while the jacket temperature and feed speed could significantly affect the alkylation, the effect of feed temperature and rotating speed on this reaction could be neglected. Under the optimal operating conditions, the conversion of TNPG and yield of 1,3,5-triethoxy-2,4,6-trinitrobenzene were 99.4 and 98.9%, respectively. Compared to the batchwise operation, alkylation of TNPG using the wiped film evaporator/distillation coupled technology is better in terms of safety, evaporation ability, productivity, and yield.

中文翻译:

使用刮膜蒸发器/蒸馏耦合技术对 1,3,5-三羟基-2,4,6-三硝基苯进行连续且安全的烷基化

1,3,5-三羟基-2,4,6-三硝基苯(TNPG)的烷基化反应是合成著名的不敏感高活性化合物2,4,6-三硝基苯-1,3,5-三胺的关键反应。 -能源材料。由于大量挥发性副产物的蒸发,在传统的搅拌反应器中进行这种烷基化具有很高的溢出和喷发事件的风险。在这项工作中,转膜蒸发器/蒸馏耦合技术用于以连续和安全的方式运行该反应。操作参数的设计基于对刮膜蒸发器的反应动力学、停留时间分布和传热能力的深入了解。结果表明,虽然夹套温度和进料速度会显着影响烷基化,进料温度和转速对该反应的影响可以忽略不计。在最佳操作条件下,TNPG的转化率和1,3,5-三乙氧基-2,4,6-三硝基苯的收率分别为99.4%和98.9%。与分批操作相比,采用转膜蒸发器/蒸馏耦合技术烷基化TNPG在安全性、蒸发能力、生产率和收率方面更佳。
更新日期:2022-08-22
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