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探索用于定制化学合成的金属和塑料3D打印光化学反应器。

Exploring metallic and plastic 3D printed photochemical reactors for customizing chemical synthesis.

作者信息

Gordeev Evgeniy G, Erokhin Kirill S, Kobelev Andrey D, Burykina Julia V, Novikov Pavel V, Ananikov Valentine P

机构信息

Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, Leninsky Prospect 47, Moscow, Russia, 119991.

Lomonosov Moscow State University, Leninskie Gory GSP-1, 1-3, Moscow, Russia, 119991.

出版信息

Sci Rep. 2022 Mar 8;12(1):3780. doi: 10.1038/s41598-022-07583-9.

Abstract

Visible light photocatalysis is a rapidly developing branch of chemical synthesis with outstanding sustainable potential and improved reaction design. However, the challenge is that many particular chemical reactions may require dedicated tuned photoreactors to achieve maximal efficiency. This is a critical stumbling block unless the possibility for reactor design becomes available directly in the laboratories. In this work, customized laboratory photoreactors were developed with temperature stabilization and the ability to adapt different LED light sources of various wavelengths. We explore two important concepts for the design of photoreactors: reactors for performing multiple parallel experiments and reactors suitable for scale-up synthesis, allowing a rapid increase in the product amount. Reactors of the first type were efficiently made of metal using metal laser sintering, and reactors of the second type were successfully manufactured from plastic using fused filament fabrication. Practical evaluation has shown good accuracy of the temperature stabilization in the range typically required for organic synthesis for both types of reactors. Synthetic application of 3D printed reactors has shown good utility in test reactions-furan C-H arylation and thiol-yne coupling. The critical effect of temperature stabilization was established for the furan arylation reaction: heating of the reaction mixture may lead to the total vanishing of photochemical effect.

摘要

可见光光催化是化学合成中一个快速发展的分支,具有显著的可持续潜力和改进的反应设计。然而,挑战在于许多特定的化学反应可能需要专门定制的光反应器才能实现最大效率。除非实验室能够直接进行反应器设计,否则这将是一个关键的绊脚石。在这项工作中,开发了定制的实验室光反应器,具有温度稳定功能,并能够适配不同波长的各种LED光源。我们探索了光反应器设计的两个重要概念:用于进行多个平行实验的反应器和适用于放大合成的反应器,从而能够快速增加产物量。第一种类型的反应器通过金属激光烧结用金属高效制成,第二种类型的反应器通过熔丝制造用塑料成功制造。实际评估表明,这两种类型的反应器在有机合成通常所需的温度范围内都具有良好的温度稳定精度。3D打印反应器的合成应用在呋喃C-H芳基化和硫醇-炔偶联等测试反应中显示出良好的实用性。对于呋喃芳基化反应,确定了温度稳定的关键作用:反应混合物的加热可能导致光化学效应完全消失。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5da5/8904794/542454aee6f3/41598_2022_7583_Fig1_HTML.jpg

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