摘要
在自制聚四氟管微通道反应器内,考察了取代芳胺重氮盐和碘化钾反应连续合成碘代芳烃的工艺过程。以碘苯为模型底物,考察了管道内径、体积流速、停留时间、反应温度等对反应的影响,得到最佳的工艺条件为:管道内径0.8 mm,体积流速1 004.8μL/min,停留时间75 s,反应温度20℃。在该条件下,碘苯产率为79.0%,时空转化率为9.41×103mol/(m3·h),比常规反应高出两个数量级。在上述最佳工艺条件下,分别研究了其他碘代芳烃在微通道反应器内的合成。
The preparation process of iodo-substituted aromatic compounds by iodination of diazonium salt and potassium iodide was investigated in self-made PTFE-microreactor. The effects of the inner diameter of microchannel reactors, flow rate, reaction time and reaction temperature on the yield were studied. The optimum conditions were determined as follows：the inner diameter of micro-channel reactors 0.8 mm, total flow rate 1 004. 8 μL/min, reaction temperature 20 ℃, reaction time 75 s. The yield of iodobenzene was 79.0% under these conditions. The STC in micro-channel reactor was 9. 41 - 103 moL/（m3 h）, more than 100 times of that in a regular reactor. The optimum reaction conditions were also applied in the preparation of other iodo-substituted aromatic compounds in microreactor.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2014年第3期397-400,408,共5页
Fine Chemicals
关键词
微通道反应器
取代芳胺
重氮盐
碘代反应
碘代芳烃
精细化工中间体
microreactor
substituent aniline
diazonium salt
iodination
iodo-substitued aromatic compounds
fine chemical intermediates
