Direct Fluorination in Mini- and Microreactors

本转移项目建立在DFG项目微反应器直接氟化的基础上。与Solvay Fluor GmbH一起，将开发、测试和应用用于直接氟化的微型和微型反应器。Woias实验室将负责设计和制造具有集成传感器技术的特别适应的微型和微型反应器。量子化学计算，以及热力学和动力学研究将在Krossing实验室进行，以便更深入地了解反应机制，并支持索尔维的后续工艺优化。此外，还将在那里进行反应器抗氟性测试，以及在实际反应条件下进行表征。该反应器技术随后将转让给Solvay Fluor GmbH，以进一步适应公司特定的研究和应用兴趣，并特别关注与现有基础设施的集成。这一过程将通过微型和微型反应器的反复设计和测试来进行。先前阶段的研究已经产生了一个具有良好特征的微型反应器以及一个完整的微反应器设计过程。完成的DFG项目是克罗辛实验室和Woias实验室之间的密切合作，其重点是直接氟化的两相微反应器的概念。这些装置和化学反应的基本行为在理论上和数值上进行了模拟，并作为设计和制造微型和微反应堆的基础。Krossing实验室在用这些反应器直接氟化有机和无机底物方面取得了重要经验，尤其侧重于循环碳酸盐。在Woias实验室进行了设计、流体模拟和制造。此外，还开发了一种基于化学镀镍的钝化技术。这种新颖的镍工艺应使用可作为微工艺工程，特别是直接氟化反应器的制造平台。该项目的目标包括：开发独立的、自支撑的金属微通道，通过与周围冷却介质直接接触来优化高度放热反应的热管理；直接集成在反应体积附近的微传感器，特别是用于过程控制的微热电偶和微压力传感器；实现反应器壁与透明段，以允许光学在线光谱。Solvay Fluor GmbH在上述环状碳酸盐的基础研究和商业生产方面有着长期的经验。迄今为止，工业合成是在经典的间歇式反应器中进行的。该项目旨在实现在连续流动微型和微反应器中对已知物质和迄今未知物质进行直接氟化的潜力。

This Transfer Project builds upon work performed in the DFG project Direct Fluorination in Microreactors. Together with Solvay Fluor GmbH, mini- and microreactors for direct fluorination will be developed, tested and applied. The Woias lab will be responsible for the design and fabrication of specifically adapted mini- and microreactors with integrated sensor technologies. Quantum chemical calculations, as well as thermodynamic and kinetic investigations will be performed in the Krossing lab in order to gain deeper insight into the reaction mechanisms and to support the following process optimization at Solvay. Also, tests of the reactor resistance to fluorine, as well as characterization under realistic reaction conditions, will be carried out there. The reactor technology will subsequently be transferred to Solvay Fluor GmbH to be further adapted for company-specific research and application interests, with a specific focus on integration into existing infrastructure. The process will be carried out via iterative design and test of both mini- and microreactors.Research in prior phases has yielded a well characterized minireactor as well as a completed microreactor design process. The completed DFG project, a close collaboration between the Krossing and Woias labs, focused on the concept of a two-phase microreactor for direct fluorination. The fundamental behavior of such devices and chemical reactions was theoretically and numerically modeled and taken as a basis for their design and fabrication as mini- and microreactors. In the Krossing lab significant experience was gained in the direct fluorination of organic and inorganic substrates with these reactors, with a particular focus on cyclic carbonates. In the Woias lab, design, fluid simulation and fabrication were performed. In addition a passivation technique was developed based on electroless nickel plating. This novel nickel technology shall be used as a fabrication platform for micro process engineering, especially for direct fluorination reactors. The project goals include: development of free-standing, self-supporting metallic microchannels for optimized thermal management of the highly exothermic reactions via direct contact with a surrounding cooling medium; direct integration of microsensors in the immediate vicinity of the reaction volume, specifically micro-thermocouples and micro-pressure sensors for process control; realization of reactor walls with transparent segments to allow for optical inline spectroscopy.Solvay Fluor GmbH has longstanding experience with the above-mentioned cyclic carbonates, both in basic research and in commercial manufacturing. To date, the commercial synthesis is performed in classical batch reactors. This project is intended to realize the potential of carrying out direct fluorination in continuous-flow mini- and microreactors, for known as well as for hitherto unknown substances.