MW Synthesis of ZIF-7. The Effect of Solvent on Particle Size and Hydrogen Sorption Properties
Vladimir A. Polyakov, Vera V. Butova, Elena A. Erofeeva, Andrei A. Tereshchenko, А. В. Солдатов
Abstract
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.