Electrosynthesis of Metal-Organic Frameworks (MOFs)Based on Nickel(II) and Benzene 1,3,5-Tri Carboxylic Acid (H3BTC): An Optimization Reaction Condition

Electrosynthesis of metal-organic frameworks based on nickel(II) and benzen 1,3,5-tricarboxylic acid (H3BTC) to form [Ni-3(BTC)(2)] has been conducted. This study aims to determine the optimum electro-synthetic conditions of [Ni-3(BTC)(2)] by varying the solvents, electrolytes, as well as the voltages. The optimum condition was determined based on the percent yield of the product which upon washing and drying at room temperature showed pale green precipitate. The materialhas high crystallinityaccording to XRD analysis with the main peak observed at 20 19 degrees and 28 degrees and appropriate with [Ni-3(BTC)(2)] pattern (CCDC No. 1274034). The refinement results using Le Bail methods revealed the Rp and Rwp values are 3.29% and 3.47%, respectively. The coordination between nickel(II) and carboxylate moeties of the linker has been characterized using FTIR and showed significant shift from 1723 cm(-1) to 1608 cm(-1). The compound has thermal stability up to 400 C according to TG/DTA analysis. The SEM analysis confirmed that compound has morphology nanoplates shape with a thickness of 75 +/- 0.023 nm. Another interesting feature of the obtained material is the occupancy of the reversible frameworks, which proved after methanol absorption. The optimum condition of the electro-synthesis of [Ni-3(BTC)(2)] achieved in the methanol with TBATFB (0.1 M) as electrolyte, and the voltage of 15 V at room temperature with a yield of 99.99%.