Abstract.A comparison synthetic strategy of Metal-Organic Frameworks, namely, Hongkong University of Techhnology-1 {HKUST-1[Cu 3 (BTC)] 2 } (BTC = 1,3,5-benzene-tri-carboxylate) through solvothermal and electrochemical method in ethanol:water (1:1) has been conducted. The obtained material was analyzed using powder X-ray diffraction, Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), Thermo-Gravimetric Analysis (TGA) and Surface Area Analysis (SAA). While the voltage in the electrochemical method are varied, ranging from 12 to 15 Volt. The results show that at 15 V the texture of the material has the best degree of crystallinity and comparable with solvothermal product. This indicated from XRD data and supported by the SEM image to view the morphology. The thermal stability of the synthesized compounds is up to 320 °C. The shape of the nitrogen sorption isotherm of the compound corresponds to type I of the IUPAC adsorption isotherm classification for microporous materials with BET surface area of 629.2 and 324.3 m²/g (for solvothermal and electrochemical product respectively) and promising for gas storage application. Herein, the methane storage capacities of these compounds are also tested.
Electro-synthesis of Metal-Organic Frameworks types of MIL-100(Fe) (MIL = Material Institute of Lavoisier) in ethanol: water (1: 1) with electrolyte TBATFB 0.1 M has been optimized by varying voltage (12, 13, 14 and 15 Volt) and temperature (room temperature, 40, 60 and 80 °C). The product showed light brown powder which upon activation becomes dark brown. Optimum condition achieved during use voltage of 15 Volts and at a temperature of 40 °C with 33% yield. The obtained material was characterized by XRD and compared to CCDC 640536 simulated patterns to confirm the phase purity of the product. As comparison hydrothermal and reflux method have been carried out. Characterization by FTIR has also undertaken to ensure the coordination between the metal cation (Fe3+) and the BTC ligand (BTC = 1,3,5-Benzene Tri Carboxylate). Meanwhile pore analysis using SAA confirmed that MIL-100(Fe) obtained by electrolysis method has a BET surface area reached till 569.191 m²/g with a total pore volume of 0.4540 cc/g and an average pore diameter reached 16 Å. Based on SEM analysis, morphology material show particle size between 0.4-8.6 μm and has a thermal stability up to 350 °C according thermo-gravimetric analysis. Due to the presence of Lewis acid sites on Fe-trimeric unit, porosity features on MIL-100(Fe) and a fairly high thermal stability, this material is potentially used as the host material for the catalyst in the conversion reactions model for green diesel production.
Abstract. (1,3,5-BTC) 2 ] (BTC = benzene-tri-carboxylate) was synthesized using an electrochemical method and tested for hydrogen storage. The obtained material showed a remarkably higher hydrogen uptake over reported HKUST-1 and reached until 4.75 wt% at room temperature and low pressure up to 1.2 bar. This yield was compared to HKUST-1 obtained from the solvothermal method, which showed a hydrogen uptake of only 1.19 wt%. Enhancement of hydrogen sorption of the electro-synthesized product was due to the more appropriate surface area and pore size, effected by the preferable physical interaction between the hydrogen gasses and the copper ions as unsaturated metal centers in the frameworks of HKUST-1.
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