Continuous synthesis of anisole in microreactor system

doi:10.11949/j.issn.0438-1157.20181246

Abstract

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

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

CLC Number:

TQ 025.5

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

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.

Figures/Tables 10

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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

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

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

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

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