Explore ways to control mechanochemical processes & scale up based on in situ data Nikita Gugin [a] , Christian Heinekamp [a,b] , Franziska Emmerling* [a,b] [a] Department Materials Chemistry, Federal Institute for Material Research and Testing, Berlin, Germany [b] Department of Chemistry, Humboldt Universität zu Berlin, Berlin, Germany
As the field of mechanochemistry continues to evolve, it has become an innovative approach to sustainable and environmentally friendly chemical and materials synthesis. [1] Despite its promise, the challenge of reproducibly scaling up mechanochemical reactions while preserving their environmental benefits remains difficult. In this context, the use of time-resolved in situ (TRIS) approaches to monitor mechanochemical reactions [2,3] offers a new and powerful way to explore and understand these transformations providing us with the necessary knowledge to unleash the potential of mechanochemistry for green materials design.
We have successfully scaled up the batch synthesis of the metal-organic framework (MOF) ZIF-8 using extrusion [4] By using an extruder to mix solid 2-methylimidazole and basic zinc carbonate in the presence of a catalytic liquid, we were able to facilitate the formation of the crystalline product. The process was optimised using a custom-designed in situ Raman spectroscopy setup investigating the influence of different parameters such as temperature, type of liquid, feed rate, and linker excess. The ball-milling synthesis of the MOF based on calcium hydroxide and terephthalic acid (Ca-MOF), studied by in situ PXRD, provided the basis for its large- scale extrusion. The effects of screw configuration, screw speed, liquid feed rate and multiple processing were investigated to maximise product yield. Our results demonstrate the potential for large-scale, environmentally friendly production of MOFs using mechanochemistry. References 1. A. A. Michalchuk, E. V. Boldyreva, A. M. Belenguer, F. Emmerling, V. V. Boldyrev, Front. Chem. 2021 , 9 , 685789. 2. A. A. Michalchuk, F. Emmerling, Angew. Chem. Int. Ed. 2022 , 61 , e202117270. 3. G. I. Lampronti, A. A. L. Michalchuk, P. P. Mazzeo, A. M. Belenguer, J. K. M. Sanders, A. Bacchi, F. Emmerling, Nat. Commun. 2021 , 12 , 6134. 4. N. Gugin, J. A. Villajos, I. Feldmann, F. Emmerling, RSC Adv. 2022 , 12 , 8940–8944.
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