Direct Fluorination in Mini- and Microreactors

小型和微反应器中的直接氟化

• 批准号: 234539006
• 负责人: Professor Dr. Ingo Krossing
• 金额: --
• 依托单位: Solvay Flour GmbH
• 依托单位国家: 德国
• 项目类别: Research Grants (Transfer Project)
• 财政年份: 2013
• 资助国家: 德国
• 起止时间: 2012-12-31 至 2016-12-31
• 项目状态: 已结题
• 来源: https://gepris.dfg.de/gepris/projekt/234539006?language=en
• 关键词: Direct; Fluorination; Mini; Microreactors

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.

该转移项目建立在DFG项目微反应器直接氟化的基础上。与索尔维氟公司一起，将开发、测试和应用用于直接脱硫的小型和微型反应器。Woias实验室将负责设计和制造具有集成传感器技术的专门适配的小型和微型反应器。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理，并支持索尔维的以下工艺优化。此外，将在那里进行反应器耐氟性测试以及在实际反应条件下的表征。该反应器技术随后将转让给索尔维氟股份有限公司，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。该过程将通过微型和微型反应器的迭代设计和测试来进行。前期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型反应器设计过程。已完成的DFG项目是Krossing和Woias实验室之间的密切合作，重点是用于直接氧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模拟，并作为其设计和制造的基础，作为小型和微型反应器。在Krossing实验室中，我们在使用这些反应器直接处理有机和无机基质方面获得了丰富的经验，特别关注环状碳酸酯。在Woias实验室中，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。这种新的镍技术将被用作微工艺工程的制造平台，特别是用于直接溅射反应器。项目目标包括：开发独立的、自支撑的金属微通道，用于通过与周围的冷却介质直接接触来优化高度放热反应的热管理;在反应体积的紧邻处直接集成微传感器，特别是用于过程控制的微热电偶和微压力传感器;实现具有透明段的反应器壁，以允许光学在线光谱。Solvay Fluor GmbH在上述环状碳酸酯方面具有长期经验，无论是在基础研究还是在商业生产中。迄今为止，商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小型和微型反应器中对已知物质以及迄今未知物质进行直接蒸馏的潜力。

项目成果

Laser rapid-prototyping and modular packaging of chip-based microreactors for direct fluorination reactions

• DOI: 10.1016/j.cherd.2017.10.017
• 发表时间: 2017-12
• 期刊: Chemical Engineering Research & Design
• 影响因子: 3.9
• 作者: Dawid Cichowski;Pengcheng Zhang;P. Woias;I. Krossing;K. Cobry

Direct Fluorination of Cyclic Carbonates andcloso-K2[B12H12] in a Slug-Flow Ministructured Reactor

团状流微型结构反应器中环状碳酸酯和closo-K2[B12H12]的直接氟化

• DOI: 10.1002/cplu.201200267
• 发表时间: 2013
• 期刊: ChemPlusChem
• 影响因子: 3.4
• 作者: M. Hill;P. Baron;K. Cobry;S. Goll;P. Lang;C. Knapp;H. Scherer;P. Woias;P. Zhang;I. Krossing
• 通讯作者: I. Krossing