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

11th Joint Conference on Chemistry in Conjunction with the 4th Regional Biomaterials Scientific Meeting

材料科学;化学;生物科学

Lestari, W.W.^1 ; Winarni, I.D.^1 ; Rahmawati, F.^1,2

Research Group of Porous Materials for Sustainability, Chemistry Department, Sebelas Maret University, Jl. Ir. Sutami 36 A, Kentingan, Jebres, Surakarta

57126, Indonesia^1

Research Group of Solid State Chemistry and Catalysis, Chemistry Department, Sebelas Maret University, Jl.Ir. Sutami 36 A, Kentingan Surakarta

57126, Indonesia^2

关键词: Drying at room temperatures;    Electro synthesis;    Metal organic framework;    Metalorganic frameworks (MOFs);    Methanol absorption;    Optimum conditions;    Reaction conditions;    Synthetic conditions;   

Others  :  https://iopscience.iop.org/article/10.1088/1757-899X/172/1/012064/pdf
DOI  :  10.1088/1757-899X/172/1/012064

来源: IOP

【 摘 要 】

Electrosynthesis of metal-organic frameworks based on nickel(II) and benzen 1,3,5-tricarboxylic acid (H3BTC) to form [Ni3(BTC)2] has been conducted. This study aims to determine the optimum electro-synthetic conditions of [Ni3(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 2θ 19° and 28° and appropriate with [Ni3(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-1to 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 [Ni3(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%.