An in situ study of resin-assisted solvothermal metal-organic framework synthesis

•Resin-assisted solvothermal MOF synthesis was studied using in situ diffraction.•Full kinetics of reaction can be obtained from in situ data.•Kinetics show that this resin-assisted synthesis is diffusion controlled.•Resin-assisted synthesis enables the production of an alternative bulk phase.

A newly developed in situ monochromatic high-energy X-ray diffraction setup was used to investigate the synthesis of MOFs using cation-impregnated polymer resin beads as a ion source. The Co–NDC–DMF (NDC=2,6-naphthalenedicarboxylate; DMF=dimethylformamide) system was investigated, a system which is known to produce at least three distinct frameworks. It was found that the resin-assisted synthesis results in the preferential formation of a topology previously impossible to synthesise in bulk, while the comparable nitrate-salt synthesis appeared to form an alternative phases. It was also found that the resin-assisted synthesis is highly diffusion-controlled.

Graphical abstractIn situ monochromatic high-energy X-ray diffraction study of a MOF synthesis.Figure optionsDownload full-size imageDownload as PowerPoint slide