微通道氯苯硝化工艺

全文下载： 20240606.pdf

文章编号： 1672-6987（2024）06-0047-09； DOI： 10.16351/j.1672-6987.2024.06.006

张效磊， 许军， 丁军委*， 张健(青岛科技大学 化工学院， 山东 青岛 266042)

摘要： 以氯苯为起始反应物，在碳化硅微通道反应器中进行混酸硝化合成一硝基氯苯。考察了氯苯与硝酸的物质的量比、硫酸与硝酸的物质的量比、预热温度、反应温度、反应停留时间等工艺参数对反应的影响，并对其进行优化。在硝酸质量分数为95%，硫酸质量分数为85%，n(氯苯)∶n(硝酸)=1∶12，n(硝酸)∶n(硫酸)=1∶21，混酸预热温度60 ℃，反应温度为85 ℃、停留时间为20 s时，氯苯转化率达到995%，一硝基氯苯收率为992%。同时对反应结束后的废酸进行再处理和多次的重复利用，提高了废酸的利用率，节约了成本。同时，在微通道反应器中进行动力学的探究，得到了反应表观活化能Ea=3343 kJ·mol-1和指数前因子A=27 90525 L·(K·mol·min)-1。该工艺反应时间大幅降低、副产物少，收率和选择性较高，更加绿色安全环保，实现了硝基氯苯的绿色安全生产，提高了生产效益。

关键词： 氯苯； 微通道反应器； 硝基氯苯； 动力学

中图分类号： TQ 612.1文献标志码： A

引用格式： 张效磊， 许军， 丁军委， 等.微通道氯苯硝化工艺［J］. 青岛科技大学学报(自然科学版), 2024, 45（6）： 47-55.

ZHANG Xiaolei， XU Jun， DING Junwei， et al.  Study on micro-channel chlorobenzene nitrification process［J］. Journal of Qingdao University of Science and Technology（Natural Science Edition), 2024， 45（6）： 47-55.

Study on  Micro-channel Chlorobenzene Nitrification Process

ZHANG Xiaolei， XU Jun， DING Junwei，  ZHANG Jian

(College of Chemical Engineering,Qingdao University of Science and Technology, Qingdao 266042, China)

Abstract: In order to obtain better production efficiency of nitrochlorobenzene and change the phenomenon of low yield and poor selectivity, chlorobenzene was used as the starting reactant to synthesize nitrochlorobenzene in a silicon carbide microchannel reactor. The effects of molar ratio of chlorobenzene to nitric acid, molar ratio of sulfuric acid to nitric acid, preheating temperature, reaction temperature and residence time on the reaction were investigated and optimized. When the mass fraction of nitric acid is 95%, the mass fraction of sulfuric acid is 85%, n(chlorobenzene)∶n(nitric acid)=1∶12, n(nitric acid)∶n(sulfuric acid)=1∶21, the preheating temperature of mixed acid is 60 ℃, the reaction temperature is 85 ℃, and the residence time is 20 s, the conversion rate of chlorobenzene is 995%, and the yield of mononitrochlorobenzene is 992%. At the same time, the waste acid after the reaction is reprocessed and reused for many times, which improves the utilization rate of waste acid and saves the cost. At the same time, the kinetics was investigated in the microchannel reactor, and the apparent activation energy Ea=3343 kJ·mol-1 and the pre-exponential factor A=27 90525 L·(K·mol·min)-1 were obtained. The process reaction time is greatly reduced, less by-products, high yield and selectivity, more green safety and environmental protection, to achieve a green and safe production of nitrochlorobenzene, improve production efficiency.

Key words: chlorobenzene; microchannel reactor; nitrochlorobenzene; dynamics

收稿日期：  2023-12-22

基金项目： 山东省重点研发计划项目（2019GSF109055）.

作者简介： 张效磊（1996—），男，硕士研究生.*通信联系人.