连续流微通道法合成新型苯乙烯阻聚剂QM-ph  

APPLICATION OF CONTINUOUS FLOW MICROCHANNEL METHOD IN SYNTHESIS OF NEW STYRENE POLYMERIZATION INHIBITOR QM-Ph

作　　者：宋启凤 赵阳 张春丽 赵甲 赵福利 Song Qifeng;Zhao Yang;Zhang Chunli;Zhao Jia;Zhao Fuli(CNOOC Ningbo Daxie Petrochemical Corporation,Ningbo 315812,Zhejiang,China;CNOOC Tianjin Chemical Research and Design Institute Co.,Ltd.,Tianjin 300131,China)

机构地区：[1]中海石油宁波大榭石化有限公司,浙江宁波315812 [2]中海油天津化工研究设计院有限公司,天津300131

出　　处：《精细石油化工》2023年第3期25-29,共5页Speciality Petrochemicals

基　　金：中国海洋石油集团有限公司科技项目(CNOOC-KJ135FZDXM00TJY005TJY2020)。

摘　　要：采用连续流微通道法,以2,6-二叔丁基苯酚和苯甲醛为原料,哌啶为催化剂合成了2,6-二叔丁基-4-苯基亚甲基-2,5-环己二烯-1-酮(QM-ph),评价了其阻聚效果。实验结果表明:适宜反应条件为n(2,6-二叔丁基苯酚)∶n(苯甲醛)∶n(哌啶)=1∶1.1∶1.05,120℃下停留30 min得到中间产物;按照m(甲酸溶液)∶m(中间产物)=1∶2.5,脱胺得到最终产物,收率达到96.4%,QM-ph的阻聚效果优于DNBP。相较于传统釜式间歇反应,连续流微通道法减少了哌啶的用量,缩短了反应时间,提高了产品收率。2,6-Di-tert-butyl-4-phenyl-methyl-2,5-cyclohexadiene-1-one(QM-ph)was synthesized using 2,6-di-tert-butylphenol and benzaldehyde as raw materials and piperidine as catalyst in a continuous flow microchannel reaction,and the polymerization inhibition effect was evaluated.The results show that the yield reaches 96.4%at optimize reaction condition:n(2,6-di-tert-butylphenol)∶n(benzaldehyde)∶n(piperidine)=1∶1.1∶1.05,stay at 120℃for 30 min to obtain intermediate products,and m(formic acid solution)∶m(intermediate products)=1∶2.5 to obtain the final product,the polymerization inhibitory effect of QM-ph is better than that of DNBP.Compared with the traditional kettle batch reaction,the continuous flow microchannel method reduces the amount of piperidine,shortens the reaction time and improves the product yield.

关 键 词：微反应器 苯乙烯阻聚剂 2 6-二叔丁基-4-苯基亚甲基-2 5-环己二烯-1-酮 

分 类 号：TQ314.244[化学工程—高聚物工业]