Electrosynthesis of coordination polymers containing magnesium(II) and benzene 1,3,5-tricarboxylate: the influence of solvents and electrolytes toward the dimensionality

• Published in: IOP conference series. Materials Science and Engineering Vol. 509; no. 1; pp. 12149 - 12159
• Main Authors: Wahyu Lestari, Witri, Shahab, Sakinah, Hikma Novita, Tria, Akbar Tedra, Rizqi, Purnawan, Candra, Fahrudin Arrozi, Ubed Sonai, Ni'maturrohmah, Dwi
• Format: Journal Article
• Language: English
• Published: Bristol IOP Publishing 03.05.2019
• Subjects: Benzene; Benzene-1,3,5-Tricarboxylate; Chemical synthesis; Coordination Polymer; Coordination polymers; Crystal structure; Crystallinity; Crystallites; Diameters; Electrolytes; electrosynthesis; Ethanol; Hydrocarbons; Magnesium; Magnesium (II); Metal-organic frameworks; Porous materials; Solvents; Thermal stability
• ISSN: 1757-8981; 1757-899X; 1757-899X
• DOI: 10.1088/1757-899X/509/1/012149

The synthesis of coordination polymers (CPs) and metal-organic frameworks (MOFs) through electrochemical method has become an interesting preference due to ease of handling, time and cost-efficient, and abundant results with high crystallinity. In this research one- and two-dimensions of CPs containing magnesium (II) and benzene 1,3,5-tricarboxylic acid (H3BTC) were successfully electro-synthesized at 15 V for 1.5 h. Reaction parameters such as solvents and electrolytes were variated and produced white crystalline materials. X-Ray diffractogram revealed that the use of 0.1 M tetrabutyl ammonium tetra-fluoroborate (TBATFB) as an electrolyte in both ethanol and ethanol: water (1:1, mol/mol) lead to the formation of 2-dimensional CP [Mg2 (BTC)(OH)(H2O)4] 2H2O (NICS-5) (NICS: National Institute of Chemistry Slovenia) . The use of 0.1 M tributyl methyl ammonium methyl sulfate (MTBS) in both ethanol and ethanol: water (1: 1) indicates conformity with the simulated pattern of [Mg3 (BTC)2(H2O)12] (NICS-4) which has a one-dimensional structure. The formation of these two compounds is further confirmed by FTIR analysis. Nitrogen sorption isotherm indicates the both compounds are non-porous materials. Compound NICS-5 synthesized in ethanol: water (1: 1) has a BET surface area of 44.243 m2/g with a total pore volume of 0.16 cc/g and an average pore diameter of 16.81Å, larger than the compound NICS-5 synthesized only in ethanol. SEM image shows that compound NICS-5 has a bigger average crystallite size than compound NICS-4. Compound NICS-5 and NICS-4 are thermally stable up to 490°C and 455°C, respectively, according to thermogravimetric measurement.