微反应器中双-(4-N,N-二甲基氨基苯基)甲烷的连续合成

The Continuous Synthesis of Bis-(4-N,N-Dimethylaminophenyl)Methane in Microreactor

以N,N-二甲基苯胺和甲醛为原料,以对氨基苯磺酸为催化剂,在微反应器中连续合成双-(4-N,N-二甲基氨基苯基)甲烷.通过对反应温度、停留时间、原料物质的量配比、催化剂用量等反应因素的考察,确定了较优的工艺参数:反应温度为120℃,停留时间为90 s,n(甲醛)∶n(N,N-二甲基苯胺)=0.6∶1.0,n(催化剂)∶n(甲醛)=3%,此时反应收率为95.2%,产品HPLC纯度为98.2%.与传统间歇釜式合成工艺相比,连续流工艺实现了双-(4-N,N-二甲基氨基苯基)甲烷合成反应的连续稳定进行,大大缩短了反应时间,适合工业化生产.

Bis(4-N,N-dimethylaminophenyl)methane is continuously synthesized by N,N-dimethylaniline with formaldehyde using p-aminobenzene sulfonic acid as catalyst in a microreactor.The optimal reaction conditions are obtained through the influences of reaction temperature,residence time,ratio of two raw materials and amount of catalyst investigated.When the reaction temperature at 120℃,residence time of 90 s,n(formaldehyde)∶n(N,N-dimethylaniline)=0.6∶1.0,amount of catalyst is 3mol%of formaldehyde,the yield of reaction is 95.2%and the purity of product is 98.2%.Compared with the traditional batch reaction process,this continuous synthesis procedure can provide the advantages such as stable reaction,shorten reaction time and suitable industrial production.