微反应器内制备4-（6-羟基己氧基）苯酚工艺

doi:10.11949/j.issn.0438-1157.20170071

化工学报 ›› 2017, Vol. 68 ›› Issue (6): 2336-2343.DOI: 10.11949/j.issn.0438-1157.20170071

• 催化、动力学与反应器 • 上一篇下一篇

微反应器内制备4-（6-羟基己氧基）苯酚工艺

李雷^1,2, 周峰^1,2, 尧超群¹, 陈光文¹

1. 中国科学院大连化学物理研究所, 辽宁大连 116023;
2. 中国科学院大学, 北京 100049

收稿日期:2017-01-16 修回日期:2017-02-25 出版日期:2017-06-05 发布日期:2017-06-05
通讯作者: 陈光文
基金资助:
国家自然科学基金项目（U1608221，U1662124）

Synthesis process of 4-(6-hydroxyhexyloxy)phenol in microreactor

LI Lei^1,2, ZHOU Feng^1,2, YAO Chaoqun¹, CHEN Guangwen¹

1. Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China;
2. University of Chinese Academy of Sciences, Beijing 100049, China

Received:2017-01-16 Revised:2017-02-25 Online:2017-06-05 Published:2017-06-05
Contact: 10.11949/j.issn.0438-1157.20170071
Supported by:
supported by the National Natural Science Foundation of China (U1608221, U1662124)

摘要/Abstract

摘要：

研究了在微反应器中利用Williamson合成法连续高效制备4-（6-羟基己氧基）苯酚的工艺过程。通过响应曲面法中的Box-Behnken模型设计实验，考察了反应温度、催化剂浓度、物料比、停留时间以及因素间的交互作用对目标产物收率的影响，并建立了响应值与影响因素之间的回归模型。根据该模型预测得到的最佳操作工艺参数为：反应温度135℃，NaOH浓度2.35 mol·L^-1，物料摩尔比2.81，停留时间2.70 min。在此条件下产物收率达79.5%，且预测值与实验值吻合良好。此外，建立了一套产物提纯方案，并通过¹H NMR谱图对产物结构进行确认。

关键词: 4-（6-羟基己氧基）苯酚, Williamson醚合成, 微反应器, 响应曲面法

Abstract:

This work mainly studied the process of producing 4-(6-hydroxyhexyloxy) phenol with Williamson synthesis in the microreactor. The Box-Behnken model in response surface methodology was used to design the experiments to investigate the effects of reaction temperature, catalyst concentration, reactant ratio, residence time, as well as the interaction among factors, on the yield. The quadratic model was established to correlate the variables to the response values. According to the model, the optimum operating parameters were determined as following temperature 135℃, the concentration of NaOH 2.35 mol·L^-1, reactant ratio 2.81, and residence time 2.70 min. Under the optimum conditions, the yield can reach 79.5%, and the error of the predicted and experimental values can be negligible, which showed the accuracy of the model. In addition, a feasible product purification method was proposed, and the structure of the product was confirmed by the ¹H NMR spectra.

Key words: 4-(6-hydroxyhexyloxy)phenol, Williamson ether synthesis, microreactor, response surface methodology

中图分类号:

TQ24

李雷, 周峰, 尧超群, 陈光文. 微反应器内制备4-（6-羟基己氧基）苯酚工艺[J]. 化工学报, 2017, 68(6): 2336-2343.

LI Lei, ZHOU Feng, YAO Chaoqun, CHEN Guangwen. Synthesis process of 4-(6-hydroxyhexyloxy)phenol in microreactor[J]. CIESC Journal, 2017, 68(6): 2336-2343.

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微反应器内制备4-（6-羟基己氧基）苯酚工艺

Synthesis process of 4-(6-hydroxyhexyloxy)phenol in microreactor

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