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[1]尚朝辉,张峰,张利雄.微反应器中硝酸硝化对叔丁基苯酚制备邻硝基对叔丁基苯酚的工艺[J].南京工业大学学报(自然科学版),2019,41(05):613-619.[doi:10.3969/j.issn.1671-7627.2019.05.011]
 SHANG Zhaohui,ZHANG Feng,ZHANG Lixiong.Preparation of 4-tert-butyl-2-nitrophenol through nitrification of 4-tert-butylphenol with nitric acid by a microreactor[J].Journal of NANJING TECH UNIVERSITY(NATURAL SCIENCE EDITION),2019,41(05):613-619.[doi:10.3969/j.issn.1671-7627.2019.05.011]
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微反应器中硝酸硝化对叔丁基苯酚制备邻硝基对叔丁基苯酚的工艺()
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《南京工业大学学报(自然科学版)》[ISSN:1671-7627/CN:32-1670/N]

卷:
41
期数:
2019年05期
页码:
613-619
栏目:
出版日期:
2019-10-22

文章信息/Info

Title:
Preparation of 4-tert-butyl-2-nitrophenol through nitrification of 4-tert-butylphenol with nitric acid by a microreactor
文章编号:
1671-7627(2019)05-0613-07
作者:
尚朝辉张峰张利雄
南京工业大学 化工学院 材料化学工程国家重点实验室,江苏 南京 211800
Author(s):
SHANG ZhaohuiZHANG FengZHANG Lixiong
State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemical Engineering, Nanjing Tech University, Nanjing 211800, China
关键词:
微反应器 对叔丁基苯酚 邻硝基对叔丁基苯酚 硝化反应
Keywords:
microreactor 4-tert-butylphenol 4-tert-butyl-2-nitrophenol nitrification reaction
分类号:
TQ243
DOI:
10.3969/j.issn.1671-7627.2019.05.011
文献标志码:
A
摘要:
针对传统硝酸硝化对叔丁基苯酚制备邻硝基对叔丁基苯酚存在生产效率低、安全性差等问题,本文发展了一种在微结构反应器中连续安全合成邻硝基对叔丁基苯酚的方法。首先,使用加热柱塞泵熔化固体对叔丁基苯酚实现连续进料,接着原料和高浓度硝酸在T形微混合器中迅速混合,再经管式反应器生成邻硝基对叔丁基苯酚。考察硝酸浓度、硝酸温度、硝酸与原料摩尔比、反应温度、停留时间以及总流速对对叔丁基苯酚转化率和邻硝基对叔丁基苯酚收率的影响。结果表明:硝酸浓度为7.5 mol/L、硝酸温度为22.4 ℃、硝酸与原料的摩尔比为1.2、反应温度90 ℃、停留时间10 s、总流速为2 mL/min为最优条件。在最优条件下,对叔丁基苯酚的转化率达到98.7%,邻硝基对叔丁基苯酚的收率达到79.9%。
Abstract:
To solve the problems such as low efficiency and low safety in traditional methods for the preparation of 4-tert-butyl-2-nitrophenol from the nitric acid nitration of 4-tert-butylphenol, a method for the continuous and safe synthesis of 4-tert-butyl-2-nitrophenol in a microstructure reactor was considered. First, continuous feeding of 4-tert-butylphenol was realized by melting solid 4-tert-butylphenol with a heated plunger pump. Then the raw material and high concentration nitric acid were reacted rapidly in the T-shape reactor to form 4-tert-butyl-2-nitrophenol. The effects of nitric acid concentration, nitric acid temperature, molar ratio of nitric acid to raw material, reaction temperature, residence time and total flow rate on the conversion of 4-tert-butyl-2-nitrophenol were investigated. Results showed that under the optimum conditions of the concentration of nitric acid of 7.5 mol/L, the temperature of nitric acid of 22.4 ℃, the molar ratio of nitric acid to raw material of 1.2, the reaction temperature of 90 ℃, the residence time of 10 s, and the total flow rate of 2 mL/min, the conversion of 4-tert-butylphenol was 98.7%, and the yield of 4-tert-butyl-2-nitrophenol was 79.9%.

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备注/Memo

备注/Memo:
收稿日期:2019-06-19
作者简介:尚朝辉(1992—),男, E-mail:shangzhaohui@yeah.net; 张利雄(联系人),教授,E-mail:lxzhangnjut@gmail.com.
引用本文:尚朝辉,张峰,张利雄.微反应器中硝酸硝化对叔丁基苯酚制备邻硝基对叔丁基苯酚的工艺[J].南京工业大学学报(自然科学版),2019,41(5):613-619..
更新日期/Last Update: 2019-09-30