MW Synthesis of ZIF-7. The Effect of Solvent on Particle Size and Hydrogen Sorption Properties

We report here fast (15 min) microwave-assisted solvothermal synthesis of zeolitic imidazolate framework material (ZIF-7). We have optimized solvent composition to achieve high porosity and hydrogen capacity and narrow particle size distribution. It was shown that synthesis in N,N-diethylformamide (DEF) results in a layered ZIF-7 III phase, while N,N-dimethylformamide (DMF) as solvent leads to a pure ZIF-7 phase in microwave conditions. A mixture of toluene with DMF allows the production of pure ZIF-7 material only with the triethylamine additive. Obtained materials were comprehensively characterized. We have pointed out that both X-ray diffraction and infrared spectroscopy could be used for the identification of ZIF-7 or ZIF-7 III phases. Although samples obtained in DMF, and in a mixture of DMF, toluene, and triethylamine were assigned to the pure ZIF-7 phase, solvent composition significantly affected the size of particles in the material and nitrogen and hydrogen adsorption process.