Direct Fluorination in Mini- and Microreactors

这一转让项目建立在DFG项目的基础上，该项目在微反应器中直接氟化。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采用集成传感器技术的专门改装的微型和微型反应堆。Krossing实验室将进行量子化学计算以及热力学和动力学研究，以便更深入地了解反应机理，并支持索尔维的后续工艺优化。此外，还将在那里进行反应堆抗氟性测试，以及在现实反应条件下的表征。反应堆技术随后将被转让给Solvay Fluor GmbH，以进一步适应公司特定的研究和应用兴趣，特别是整合到现有基础设施中。这一过程将通过微型和微型反应堆的迭代设计和测试来进行。前几个阶段的研究已经产生了一个具有良好特性的微型反应器以及一个完整的微型反应器设计过程。完成的DFG项目是Krossing和Woias实验室之间的密切合作，重点是用于直接氟化的两相微反应器的概念。对这种装置和化学反应的基本行为进行了理论和数值模拟，并将其作为设计和制造微型和微反应器的基础。在Krossing实验室，这些反应器在有机和无机底物的直接氟化方面获得了丰富的经验，特别是在环状碳酸盐方面。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工艺。这项新的镍技术将作为微工艺工程，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、自持的金属微通道，用于通过与周围冷却介质的直接接触来优化高放热反应的热管理；直接集成反应体积附近的微传感器，特别是用于过程控制的微型热电偶和微压力传感器；实现带有透明段的反应堆壁，以便进行光学在线光谱分析。到目前为止，商业合成是在经典的间歇反应器中进行的。该项目旨在实现在连续流动微型和微反应器中进行直接氟化的潜力，已知的和迄今未知的物质也是如此。

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.