以2-氨基-4-硝基苯酚为重氮组分、β-萘酚为偶合组分,利用具有脉冲混合结构的微通道反应器进行连续偶合反应;考察了反应温度、反应时间、盐酸的用量对重氮化反应的影响,以及反应温度、反应时间、反应体系pH对偶合反应的影响。通过实验确定了较优的工艺条件为:2-氨基-4-硝基苯酚与β-萘酚摩尔比为1:1.01、反应温度为20℃、助剂1与β-萘酚的质量比为3:1、反应体系pH为6,该条件下反应的总收率为98.0%。研究结果表明,与间歇法相比,连续流工艺使反应时间缩短了近80%,反应收率提高了近5%,有利于降低原料消耗和工艺过程的能耗,提高生产效率。

With 2-amino-4-nitrophenol as diazo component and β-naphthol as coupling component,continuous coupling reaction is carried out in a microchannel reactor with pulse mixing structure.The influences of reaction temperature,reaction time and the adding amount of hydrochloric acid on diazotization reaction are studied,and the effects of reaction temperature,reaction time and pH value of reaction system on coupling reaction are investigated.Through experiments,the optimum process conditions are determined as follows:the molar ratio of 2-amino-4-nitrophenol to β-naphthol is 1:1.01,the reaction temperature is 20℃,the mass ratio of assistant 1 to β-naphthol is 3:1,and the pH value of the reaction system is 6.Under these conditions,the total yield is 98.0%.Compared with the batch process,the continuous flow process shortens the reaction time by nearly 80% and increases the reaction yield by nearly 5%,which is conducive to reducing the raw materials consumption and energy consumption in the process and improving the production efficiency.

王鹏(1997-),男,硕士研究生,研究方向为连续流化工工艺开发,1076772159@qq.com