邻二氯苯合成3,4-二氯硝基苯的连续流工艺研究

马凯旋, 张跃, 严生虎, 刘建武, 沈介发, 马晓明, 辜顺林, 陈代祥

现代化工 ›› 2020, Vol. 40 ›› Issue (8) : 154 -157.

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现代化工 ›› 2020, Vol. 40 ›› Issue (8) : 154-157. DOI: 10.16606/j.cnki.issn0253-4320.2020.08.032
科研与开发

邻二氯苯合成3,4-二氯硝基苯的连续流工艺研究

    马凯旋, 张跃, 严生虎, 刘建武, 沈介发, 马晓明, 辜顺林, 陈代祥
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Continuous flow process for synthesis of 3,4-dichloronitrobenzene from o-dichlorobenzene

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摘要

以邻二氯苯为原料、硝酸为硝化剂、浓硫酸为溶剂,研究了在脉冲混合结构微通道反应器中合成3,4-二氯硝基苯的连续流工艺,考察了反应物料摩尔比、硝硫混酸摩尔比、反应温度、反应停留时间等工艺条件。结果表明,当n(邻二氯苯)∶n(硝酸)∶n(硫酸)=1∶2∶4、反应体系温度为60℃、停留时间为135 s时,反应效果最佳。该工艺充分利用了微通道反应器优良的传质传热特点,缩短了反应时间,扩大了工艺条件选择区间,实现了对反应过程的有效控制,增加了安全系数。

Abstract

The continuous flow process for synthesizing 3,4-dichloronitrobenzene in pulse mixed structure microchannel reactor is studied by using o-dichlorobenzene as raw material,nitric acid as nitrating agent and concentrated sulfuric acid as solvent.Through studying the molar ratio of reactive materials,the molar ratio of nitric acid to sulfuric acid,the reaction temperature,the residence time etc.,the optimum process conditions are obtained as follows:n(o-dichlorobenzene):n(nitric acid):n(sulfuric acid)=1:2:4,the reaction system temperature is at 60℃,and the residence time is 135 s.This process fully utilizes the excellent mass transfer and heat transfer characteristics of the microchannel reactor,greatly shortens the reaction time,increases the reaction rate,expands the selection interval of the process conditions,realizes effective control of the reaction process,and increases the safety factor.

关键词

邻二氯苯 / 连续流工艺 / 微通道反应器 / 浓硫酸 / 硝酸

Key words

o-dichlorobenzene / continuous flow process / microchannel reactor / concentrated sulfuric acid / nitric acid

Author summay

马凯旋(1995-),男,硕士研究生,研究方向为医药中间体合成,1609560124@qq.com

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邻二氯苯合成3,4-二氯硝基苯的连续流工艺研究[J]. 现代化工, 2020, 40(8): 154-157 DOI:10.16606/j.cnki.issn0253-4320.2020.08.032

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