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http://dx.doi.org/10.14478/ace.2021.1078

Optimization of MOF-801 Synthesis Using Sequential Design of Experiments  

Lee, Min Hyung (Department of Chemical & Biomolecular Engineering, Seoul National University of Science and Technology)
Yoo, Kye Sang (Department of Chemical & Biomolecular Engineering, Seoul National University of Science and Technology)
Publication Information
Applied Chemistry for Engineering / v.32, no.6, 2021 , pp. 621-626 More about this Journal
Abstract
A sequential design of experiments was used to optimize MOF-801 synthesis process. For the initial screening, a general 2k factorial design was selected followed by the central composition design, one of the response surface methods. A 23 factorial design based on the molar ratio of fumaric acid, dimethylformamide (DMF), and formic acid was performed to select the more suitable response variable for the design of experimental method among the crystallinity and BET specific surface area of MOF-801. After performing 8 synthesis experiments designed by MINITAB 19 software, the characteristic analysis was performed using XRD analysis and nitrogen adsorption method. The crystallinity with R2 = 0.999 was found to be more suitable for the experimental method than that of BET specific surface area. Based on analysis of variance (ANOVA), it was confirmed that the molar ratio of fumaric acid and formic acid was a major factor in determining the crystallinity of MOF-801. Through the response optimization and contour plot of two factors, the optimal molar ratio of ZrOCl2·8H2O : fumaric acid : DMF : formic acid was 1 : 1 : 39 : 35. In order to optimize the synthesis process, the central composition design on synthesis time and temperature was performed under the identical molar ratio of precursors. The results derived through the designed 9 synthesis experiments were calculated using the quadratic model equation. Thus, the maximum crystallinity of MOF-801 predicted under the synthesis time and temperature of 7.8 h and 123 ℃, respectively.
Keywords
Sequential design of experiments; MOF-801; Synthesis optimization;
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