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

13th Joint Conference on Chemistry

Lestari, Witri Wahyu^1 ; Shahab, Sakinah^1 ; Novita, Tria Hikma^1 ; Tedra, Rizqi Akbar^1 ; Purnawan, Candra^1 ; Arrozi, Ubed Sonai Fahrudin^2 ; Ni'Maturrohmah, Dwi^1

Chemistry Department, Faculty of Mathematics and Natural Sciences, Sebelas Maret University, Jebres, Surakarta, Indonesia^1

Department of Inorganic Chemistry, Dresden University of Technology, Mommsenstrasse 6, Dresden

01069, Germany^2

关键词: Coordination Polymers;    ELectrochemical methods;    electrosynthesis;    Metalorganic frameworks (MOFs);    Nitrogen sorption isotherms;    One-dimensional structure;    Thermogravimetric measurement;    X-ray diffractograms;   

Others  :  https://iopscience.iop.org/article/10.1088/1757-899X/509/1/012149/pdf
DOI  :  10.1088/1757-899X/509/1/012149

来源: IOP

【 摘 要 】

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.