Integrated Flow Emulsion Electrosynthetic System by In Situ Generation of Emulsions, Subsequent Emulsion Electrolysis, and Final Phase Separation

Integrated Flow Emulsion Electrosynthetic System by In Situ Generation of Emulsions, Subsequent Emulsion Electrolysis, and Final Phase Separation
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通过原位生成乳液、随后的乳液电解和最终相分离的集成流乳液电合成系统

DOI:
10.1021/acs.oprd.2c00004
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发表时间:
2022
期刊:
Organic Process Research & Development
影响因子:
--
通讯作者:
Atobe Mahito
Atobe Mahito
中科院分区:
--
文献类型:
--
作者:
Mikami Rio;Shida Naoki;Atobe Mahito

文献摘要

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本工作中,我们开发了一个连续流乳液电解系统。这种新的流动系统涉及20 kHz的超声波处理的水不溶性有机胺在水性电解质中的声乳化,而不使用表面活性剂,然后通过乳液电解在流动微反应器和分离的乳液成水和油产品(有机腈)相使用液-液分离器。20 kHz超声处理提供了稳定的乳化溶液,其含有在微米范围内具有相对窄的尺寸分布的有机胺液滴。随后在微反应器中的乳液电解非常有效地产生所需的腈产物。另外,在连续流操作中,使用液-液分离器将电解后的乳液有效地分离成水性电解质和油产物。所提出的系统是鲁棒的,并且在克规模下成功地合成了所需的产物。
In this work, we developed a continuous flow emulsion electrosynthetic system. This new flow system involves 20 kHz ultrasonication for acoustic emulsification of water-insoluble organic amines in an aqueous electrolyte without the use of a surfactant, followed by emulsion electrolysis in the flow microreactor and separation of the emulsion into aqueous and oil product (organic nitriles) phases using a liquid–liquid separator. The 20 kHz ultrasonication provided a stable emulsified solution containing organic amine droplets with a relatively narrow size distribution in the micrometer range. The subsequent emulsion electrolysis in the microreactor yielded the desired nitrile product very effectively. In addition, in a continuous flow operation, the emulsion after the electrolysis was efficiently separated into an aqueous electrolyte and oil product using a liquid–liquid separator. The proposed system is robust, and the desired product was successfully synthesized at the gram scale.