微反应器内苯甲醚连续合成

doi:10.11949/j.issn.0438-1157.20181246

化工学报 ›› 2019, Vol. 70 ›› Issue (3): 922-928.DOI: 10.11949/j.issn.0438-1157.20181246

• 催化、动力学与反应器 • 上一篇下一篇

微反应器内苯甲醚连续合成

王瀚琳¹(),王德强²(),王凯¹(),骆广生¹

1. 清华大学化学工程系，化学工程联合国家重点实验室，北京 100084
2. 山东半岛卤水资源高值化绿色化综合利用工程;技术研究中心，山东潍坊 262700

收稿日期:2018-10-22 修回日期:2018-12-28 出版日期:2019-03-05 发布日期:2019-03-05
通讯作者: 王德强,王凯
作者简介:<named-content content-type="corresp-name">王瀚琳</named-content>（1996—），男，本科生，<email>wanghl14@mails.tsinghua.edu.cn</email>|王德强（1973—），男，博士，讲师，<email>ciacwdq@163.com</email>|王凯（1983—），男，博士，副教授，<email>kaiwang@tsinghua.edu.cn</email>
基金资助:
国家自然科学基金项目(21776150)

Continuous synthesis of anisole in microreactor system

Hanlin WANG¹(),Deqiang WANG²(),Kai WANG¹(),Guangsheng LUO¹

1. Department of Chemical Engineering, State Key Laboratory of Chemical Engineering, Tsinghua University, Beijing 100084, China
2. Shandong Peninsula Engineering Research Center of Comprehensive Brine Utilization, Weifang University of Science and Technology，Weifang 262700, Shandong, China

Received:2018-10-22 Revised:2018-12-28 Online:2019-03-05 Published:2019-03-05
Contact: Deqiang WANG,Kai WANG

摘要/Abstract

摘要：

苯甲醚是一种重要的溶剂和有机合成中间体，以往通过间歇反应合成，存在生产效率低下、操作周期长等问题，亟需开发连续化的生产装置和技术。提出以苯酚钠水溶液和硫酸二甲酯为原料通过连续微反应器合成苯甲醚的方法。该方法利用微混合器和局部收缩的反应管道强化反应物的混合，在近似绝热的反应条件下快速完成反应过程。报道了苯酚钠浓度、反应物流量和反应物摩尔比对于微反应器内苯酚钠转化率和硫酸二甲酯利用率的影响规律。与文献报道的间歇反应进行了对比，揭示了微反应技术的优势。

关键词: 苯甲醚, 微反应器, 混合, 流动, 合成, 连续操作

Abstract:

Anisole is an important solvent and organic synthesis inter20181246te. In the past, it was synthesized by batch reaction, which has problems such as low production efficiency and long operation cycle. A continuous synthesis device and technology for anisole is highly required. A continuous-flow microreaction method using sodium phenolate solution and dimethyl sulfate as reactants was proposed. The microreactor employs micromixer and locally constructive reaction tube to enhance reactant mixing and the reaction was carried out at approximately adiabatic condition. The influences of sodiumphenolate concentration, reactant flow rate and molar ratio of phenolatetodimethyl sulfate on the sodium phenolate conversion and dimethyl sulfate utility were reported. A comparison with the batch reaction in the literatures was provided to show the advantage of microreaction technology.

Key words: anisole, microreactor, mixing, flow, synthesis, continuous operation

中图分类号:

TQ 025.5

王瀚琳, 王德强, 王凯, 骆广生. 微反应器内苯甲醚连续合成[J]. 化工学报, 2019, 70(3): 922-928.

Hanlin WANG, Deqiang WANG, Kai WANG, Guangsheng LUO. Continuous synthesis of anisole in microreactor system[J]. CIESC Journal, 2019, 70(3): 922-928.

图/表 10

图1 苯甲醚微反应器连续合成装置

Fig.1 Schematic diagram of continuous synthesis of anisole using microreactor

图2 反应管道出口液滴分散状况（实验条件：Q T = 28.3 ml·min-1，n PhONa,0/n DMS,0 = 1）

Fig.2 Dispersion of droplets from outlet of reaction tube

图3 沿反应管道的温度分布

Fig.3 Temperature distribution along reaction tube

表1 反应时间与进料流量的关系

Table 1 Relation between reaction time and flow rate

Q _T /(ml·min^-1)	T _max /℃	T _max管道位置/m	反应时间/min
2.83	74.9	7	7.77
5.66	83.1	9	2.50
11.3	89.9	9	1.66
22.6	94.9	9	1.25
28.3	97.7	9	1.00
33.8	95.6	9	0.84
45.3	94.3	11	0.76

图4 物料流量对苯酚钠转化率的影响

Fig.4 Effect of flow rate on sodium phenolate conversion

图5 进料摩尔比对反应的影响

Fig.5 Effects of molar feed ratio of reactants on reaction

表2 苯酚钠浓度对其转化率和硫酸二甲酯利用率的影响

Table 2 Effect of sodium phenolate concentration on its conversion and DMS utility

n _PhONa,0/n _DMS,0	PhONa质量分数/%	w _PhONa/%	y _DMS/%
1.0	20	56.6	56.6
0.9	20	57.8	52.0
0.8	20	59.6	47.7
1.0	30	80.4	80.4
0.9	30	82.4	74.2
0.8	30	86.4	69.1
1.0	40	89.2	89.2
0.9	40	93.5	84.2
0.8	40	93.6	74.9

表3 重复性实验结果

Table 3 Results of repeated experiments

参数	实验条件 1	实验条件2
PhONa质量分数/%	30	40
n _PhONa,0/n _DMS,0	1.0	0.8
Q _T/(ml·min^-1)	28.3	28.3
w _PhONa/%	80.9,81.3,80.4	93.6,93.5
y _DMS/%	80.9,81.3,80.4	74.9,74.8

表4 苯甲醚间歇法合成收率[14]

Table 4 Yield for batch synthesis of anisole[14]

操作时间/h	DMS/mol	PhOH/mol	NaOH/mol	PhONa质量分数/%	w _PhONa/%
1	0.1	0.2	0.3	38.9	54.6
1	0.1	0.2	0.3	26.2	39.3

图6 反应物在管道内的停留时间

Fig.6 Residence time of reactants in reaction tube

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微反应器内苯甲醚连续合成

Continuous synthesis of anisole in microreactor system

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