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Development of Lab-Scale Continuous Stirred-Tank Reactor as Flow Process Tool for Oxidation Reactions Using Molecular Oxygen
Organic Process Research & Development ( IF 3.4 ) Pub Date : 2024-05-08 , DOI: 10.1021/acs.oprd.3c00424
Ursina Gnädinger 1 , Dario Poier 1 , Claudio Trombini 2 , Michal Dabros 1 , Roger Marti 1
Affiliation  

The use of sustainable oxidants is of great interest to the chemical industry, considering the importance of oxidation reactions for the manufacturing of chemicals and society’s growing awareness of its environmental impact. Molecular oxygen (O2), with an almost optimal atom efficiency in oxidation reactions, presents one of the most attractive alternatives to common reagents that are not only toxic in most cases but produce stoichiometric amounts of waste that must be treated. However, fire and explosion safety concerns, especially when used in combination with organic solvents, restrict its easy use. Here, we use state-of-the-art 3D printing and experimental feedback to develop a miniature continuous stirred-tank reactor (mini-CSTR) that enables efficient use of O2 as an oxidant in organic chemistry. Outstanding heat dissipation properties, achieved through integrated jacket cooling and a high surface-to-volume ratio, allow for a safe operation of the exothermic oxidation of 2-ethylhexanal, surpassing previously reported product selectivity. Moving well beyond the proof-of-concept stage, we characterize and illustrate the reactor’s potential in the gas–liquid–solid triphasic synthesis of an endoperoxide precursor of antileishmanial agents. The custom-designed magnetic overhead stirring unit provides improved stirring efficiency, facilitating the handling of suspensions and, in combination with the borosilicate gas dispersion plate, leading to an optimized gas–liquid interface. These results underscore the immense potential that lies within the use of mini-CSTR in sustainable chemistry.

中文翻译:

开发实验室规模的连续搅拌釜反应器作为使用分子氧的氧化反应的流程工具

考虑到氧化反应对于化学品制造的重要性以及社会对其环境影响的日益认识,化学工业对可持续氧化剂的使用非常感兴趣。分子氧 (O 2 ) 在氧化反应中具有几乎最佳的原子效率,是常见试剂最有吸引力的替代品之一,这些试剂不仅在大多数情况下有毒,而且会产生必须处理的化学计量量的废物。然而,火灾和爆炸安全问题,特别是与有机溶剂结合使用时,限制了其易用性。在这里,我们使用最先进的 3D 打印和实验反馈来开发微型连续搅拌釜反应器 (mini-CSTR),能够在有机化学中有效利用 O 2作为氧化剂。通过集成夹套冷却和高表面积体积比实现出色的散热性能,可实现 2-乙基己醛放热氧化的安全操作,超越了之前报道的产品选择性。远远超出了概念验证阶段,我们描述并说明了反应器在抗利什曼尼制剂的内过氧化物前体的气-液-固三相合成中的潜力。定制设计的磁力顶置搅拌装置可提高搅拌效率,促进悬浮液的处理,并与硼硅酸盐气体分散板结合使用,实现优化的气液界面。这些结果强调了微型 CSTR 在可持续化学中的应用的巨大潜力。
更新日期:2024-05-08
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