Synthesis of a CE-based MOF-76 with high yield: A study of reaction parameters based on a factorial design

Abstract

The purpose of this work was to optimize the synthesis yield of {[Ce(BTC)(H2O)]·DMF}n, a metal-organic framework (MOF)-76 family member, by solvothermal method. CeCl3.7H2O and 1,3,5-benzenetricarboxylic acid, 2:1 molar proportion, were added to N,N-dimethylformamide (DMF). Reaction time and temperature were evaluated to optimize the synthesis through a factorial design followed by a statistical analysis of the response variable (reaction yield). Infrared spectroscopy (IR), X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) analyses were performed to characterize the obtained white powders. Reaction yield was estimated based on {[Ce(BTC)(H2O)]·DMF}n molecular formula, which was confirmed by analytical techniques. The proposed statistic model of the response variable showed good agreement with the experimental values. Temperature parameter was the only significant variable on the reaction yields, being the highest yield (94.4%) obtained at 115 °C for 36 h, and it was accompanied by an improvement on the particle morphology (uniformity of shape and size), forming particles with strawsheave-like morphology.