化学
苯甲酸
混合(物理)
体积流量
微型反应器
阿累尼乌斯方程
反应速率
间歇式反应器
干扰素
热力学
连续反应器
停留时间(流体动力学)
反应性(心理学)
烷基化
流动化学
推流式反应器模型
塞流
分析化学(期刊)
连续搅拌釜式反应器
有机化学
物理化学
活化能
催化作用
医学
物理
明渠流量
量子力学
岩土工程
湍流
替代医学
病理
工程类
作者
Christophe Penverne,Benjamin Hazard,Christian Rolando,Maël Penhoat
标识
DOI:10.1021/acs.oprd.7b00246
摘要
The esterification reaction is one of the most important reaction in organic chemistry, and the development of scalable continuous flow conditions is of high interest. Here we describe a scaling-up study of benzoic acid alkylation by MeI in the presence of superbases from a capillary reactor (282 mg·h–1 at 75 °C) to a low flow reactor (LFR, 6.82 g·h–1 at 80 °C). First, the optimization of the base demonstrated that 1,8-diazabicyclo[5.4.0]-undec-7-ene (DBU) was a good compromise in terms of basicity and price. A comparison between batch and LFR reaction showed similar kinetic rates. We also observed a maximum reactivity for a flow rate of 3 mL·min–1 which corresponds to an optimum mixing of the entering fluids. A colorimetric study permits to show a visual change in the flow regime (dispersed to stratified) by varying the flow rate with a maximum conversion obtained at 3 mL·min–1 corresponding to a 105 s residence time, demonstrating that the studied reaction is sensitive to mixing conditions and that LFR presents some mixing limitations for low flow rates. After thermal optimization (80 °C), the reaction has been improved to a productivity of 6.82 g/h at the lab scale using DBU as the base and Eyring/Arrhenius plots permitted to extract activation energies.
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