Mechanochemistry is quickly becoming a viable, sometimes even superior alternative to traditional solution synthesis. Its benefits include avoiding bulk solvent, high atom economy, room temperature reactivity, and higher yields in a shorter time. Applications of mechanochemistry range from nanoparticle synthesis to organic, inorganic and metal-organic chemistry, sometimes giving products traditional synthesis can not attain. However, the benefits of mechanochemistry are often disregarded by the wider chemical comunity due to poor understanding of its mechanisms. Recently, the first real-time observations of mechanochemical reactions were reported, using synchrotron X-ray powder diffraction and/or Raman spectroscopy, greatly advancing the understanding of mechanisms behind ball milling transformations. We now demonstrate the change in pressure within the reaction vessel as a means for real-time monitoring of the mechanochemical assembly of the commercially relevant microporous framework ZIF-8 from basic zinc carbonate. In particular, the release of CO2 gas during the reaction of the carbonate with an imidazole reactant provided direct insight into the reaction kinetics, yield, and revealed a reaction byproduct, facilitating the optimization of reaction conditions for ZIF-8 synthesis.

In situand real-time monitoring of mechanochemical ZIF8 synthesis via gas pressure measurements

253rd National Meeting (2017)

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