In this study,a continuous-flow procedure containing four steps has been developed to synthesize Pigment Red 53 and modify its crystal structure.This process avoided the problems of conveying highly insoluble reaction...In this study,a continuous-flow procedure containing four steps has been developed to synthesize Pigment Red 53 and modify its crystal structure.This process avoided the problems of conveying highly insoluble reaction intermediates by removing intermediate operating steps.After optimization,the overall yield of Pigment Red 53:1 reached 97.1%in the total residence time of 80 s by this diazotizationcoupling-laking-crystal transition process.From batch to continuous flow,the purity of products increased from 97.1%to 98.2%and the median diameter of pigment particles decreased from 14μm to 1.9μm.This process achieved a similar crystal transition effect in 18 s as in batch,producingα,δandνcrystals of Pigment Red 53:2 as expected.In conclusion,this continuous-flow procedure displays advantages in both synthesis and crystal transition,indicating another potential use for industrial application.展开更多
基金financial support from Shanghai Municipal Science and Technology Commission (No.21520761100)the Open Project of State Key Laboratory of Chemical Engineering (No. SKL-Ch E-21C07)+1 种基金the Fundamental Research Funds for the Central Universitiesthe Program of Leading Talents (2013)
文摘In this study,a continuous-flow procedure containing four steps has been developed to synthesize Pigment Red 53 and modify its crystal structure.This process avoided the problems of conveying highly insoluble reaction intermediates by removing intermediate operating steps.After optimization,the overall yield of Pigment Red 53:1 reached 97.1%in the total residence time of 80 s by this diazotizationcoupling-laking-crystal transition process.From batch to continuous flow,the purity of products increased from 97.1%to 98.2%and the median diameter of pigment particles decreased from 14μm to 1.9μm.This process achieved a similar crystal transition effect in 18 s as in batch,producingα,δandνcrystals of Pigment Red 53:2 as expected.In conclusion,this continuous-flow procedure displays advantages in both synthesis and crystal transition,indicating another potential use for industrial application.