[1]芮培欣,许招会,郭晓红,等.微反应器中双-(4-N,N-二甲基氨基苯基)甲烷的连续合成[J].江西师范大学学报(自然科学版),2020,(02):174-177.[doi:10.16357/j.cnki.issn1000-5862.2020.02.11]
　RUI Peixin,XU Zhaohui,GUO Xiaohong,et al.The Continuous Synthesis of Bis-(4-N,N-Dimethylaminophenyl)Methane in Microreactor[J].Journal of Jiangxi Normal University:Natural Science Edition,2020,(02):174-177.[doi:10.16357/j.cnki.issn1000-5862.2020.02.11]
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微反应器中双-(4-N,N-二甲基氨基苯基)甲烷的连续合成()
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《江西师范大学学报》（自然科学版）[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2020年02期
页码:
174-177
栏目:
化学与生命科学
出版日期:
2020-04-10

文章信息/Info

Title:
The Continuous Synthesis of Bis-(4-N,N-Dimethylaminophenyl)Methane in Microreactor
文章编号:
1000-5862(2020)02-0174-04
作者:
芮培欣; 许招会; 郭晓红; 胡石金; 廖维林*
江西师范大学国家单糖化学合成工程技术研究中心,江西 南昌 330027
Author(s):
RUI Peixin; XU Zhaohui; GUO Xiaohong; HU Shijin; LIAO Weilin*
National Monosaccharide Chemical Synthesis Engineering Research Center,Jiangxi Normal University,Nanchang Jiangxi 330022,China
关键词:
双-(4-N; N-二甲基氨基苯基)甲烷;  N; N-二甲基苯胺;  甲醛;  微反应器;  连续合成
Keywords:
bis(4-N; N-dimethylaminophenyl)methane;  N; N-dimethylaniline;  formaldehyde;  microreactor;  continuous synthesis
分类号:
O 624; TQ 246.3
DOI:
10.16357/j.cnki.issn1000-5862.2020.02.11
文献标志码:
A
摘要:
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.
Abstract:
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.

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备注/Memo

备注/Memo:
收稿日期:2019-11-04
基金项目:国家重点研发计划(2017YFB0404300)和江西省教育厅科学技术研究(GJJ160291)资助项目.
通信作者:廖维林(1963-),男,江西抚州人,教授,博士生导师,主要从事精细化学品的研究.E-mail:44330684@qq.com
更新日期/Last Update: 2020-04-10