文献类型：期刊文献

英文题名：Effective Phosphorylation of 2,2′-Methylene-bis(4,6-di-tert-butyl) Phenol in Continuous Flow Reactors

作者：Yao, Hanlin[1];Li Wan[1];Zhao, Xiaoyu[1];Guo, Yahui[1];Zhou, Jian[1];Bo, Xiaofan[1];Mao, Yuxin[1];Xin, Zhong[1,2]

机构：[1]East China Univ Sci & Technol, Sch Chem Engn, Shanghai Key Lab Multiphase Mat Chem Engn, Shanghai 200237, Peoples R China;[2]East China Univ Sci & Technol, Sch Chem Engn, State Key Lab Chem Engn, Shanghai 200237, Peoples R China

年份：2021

卷号：25

期号：9

起止页码：2060

外文期刊名：ORGANIC PROCESS RESEARCH & DEVELOPMENT

收录：;EI(收录号：20213610874257);WOS:【SCI-EXPANDED(收录号:WOS:000697356700006)】；

基金：The authors would like to acknowledge financial support from the Innovation Program of Shanghai Municipal Education Commission (2019-01-07-00-02-E00061), the Fundamental Research Funds for the Central Universities (50321011917025 and 50321011918010), and the Program of Leading Talents (2013).

语种：英文

外文关键词：phosphorylation reaction; continuous flow synthesis; precipitation clogging; process optimization; reactor analysis

摘要：Nucleating agent intermediate 2,2'methylene-bis(4,6-di-tert-butylphenol) phosphate chloride was synthesized successfully in a continuous flow by the phosphorylation reaction for the first time. After evaluating several different continuous flow reactors, the continuous Coflore agitated cell reactor (ACR) designed based on the continuous stirred-tank reactor (CSTR) principle was proved capable of overcoming the severe channel clogging caused by the precipitation product triethylamine hydrochloride. This can be attributed to the violent agitation and particle size control by the moving agitators. The yield in continuous flow after optimization reached nearly 98% at 100 degrees C within the residence time of only 4 min and the optimal equivalents of triethylamine and POCl3 are 2.8 and 1.1, respectively. In contrast to the batch operation, the yield has been increased through continuous operation. This is an effective method for the synthesis of the desired product and exhibits the merits of short residence time, easy operation, and straightforward scale-up.