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

doi:10.11949/j.issn.0438-1157.20170071

Abstract

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

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

CLC Number:

TQ24

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.

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.

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