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- In relation to this article, we declare that there is no conflict of interest.
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Received November 14, 2022
Revised December 19, 2022
Accepted January 13, 2023
- Acknowledgements
- This study was supported by the Research Program funded by the SeoulTech (Seoul National University of Science and Technology).
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Evaluation of Design of Experiments to Develop MOF-5 Adsorbent for Acetylene Capture
1Department of Energy & Chemical Engineering, Graduate School of Convergence Science, Seoul National University of Science and Technology, Seoul, 01811, Korea 2Department of Chemical & Biomolecular Engineering, Seoul National University of Science and Technology, Seoul, 01811, Korea
kyoo@seoultech.ac.kr
Korean Chemical Engineering Research, May 2023, 61(2), 322-327(6), 10.9713/kcer.2023.61.2.322 Epub 31 May 2023
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Abstract
A design of experiments was evaluated in optimizing MOF-5 synthesis for acetylene adsorption. At first,
mixture design was used to optimize precursor concentration, terephthalic acid, zinc acetate dihydrate and N,Ndimethylformamide. More specifically, 13 conditions with various molar ratios were designed by extreme vertices
design method. After preparing the samples, XRD, N2 physisorption and SEM analysis were performed for their
characterization. Moreover, acetylene adsorption experiments were carried out over the samples under identical conditions.
The optimal precursor composition for MOF-5 synthesis was predicted on a molar basis as follows: terephthalic acid :
acetate dihydrate : dimethylformamide = 0.1 : 0.4 : 0.5. Thereafter, multi-level factorial design was designated to
investigate the effect of synthesis reaction conditions such as temperature, time and stirring speed. By the statistical
analysis of 18 samples designed, 4 reaction parameters were determined for additional adsorption experiments. Therefore,
MOF-5 prepared under the synthesis time and temperature of 100 ℃ and 12 h, respectively, showed the maximum
adsorption capacity of 15.1 mmol/g.
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2. Breck, D. W., Eversole, W. G., Milton, R. M., Reed, T. B. and Thomas, T. L., “Crystalline Zeolites. I. The Properties of a New Synthetic Zeolite, Type A,” J. Am. Chem. Soc., 78, 5963-5972(1956).
3. Amaro, A. A. and Seff, K., “Crystal Structure of an Acetylene Sorption Complex of Zeolite 4A,” J. Phys. Chem.,77, 906-910(1973).
4. Reid, C. R. and Thomas, K. M., “Adsorption of Gases on a Carbon Molecular Sieve Used for Air Separation: Linear Adsorptives as Probes for Kinetic Selectivity,” Langmuir, 15, 3206-3218(1999).
5. Newalkar, B. L., Choudary, N. V., Kumar, P., Komarneni, S. and Bhat, T. S. G., “Exploring the Potential of Mesoporous Silica,SBA-15, as an Adsorbent for Light Hydrocarbon Separation,”Chem. Mater., 14, 304-309(2002).
6. Newalkar, B. L., Choudary, N. V., Turaga, U. T., Vijayalakshmi,R. P., Kumar, P., Komarneni, S. and Bhat, T. S. G., “Adsorption of Light Hydrocarbons on HMS Type Mesoporous Silica,”Micropor. Mesopor. Mater., 65, 267-276(2003).
7. Eddaoudi, M., Moler, D. B., Li, H., Chen, B., Reineke, T. M.,O’Keeffe, M. and Yaghi, O. M., “Modular Chemistry: Secondary Building Units as a Basis for the Design of Highly Porous and Robust Metal-organic Carboxylate Frameworks,” Acc. Chem. Res.,34, 319-330(2001).
8. Eddaoudi, M., Kim, J., Rosi, N. L., Vodak, D., Wachter, J., O'Keeffe,M. and Yaghi, O. M., “Systematic Design of Pore Size and Functionality in Isoreticular MOFs and Their Application in Methane Storage,” Science, 295, 469-472(2002).
9. Ockwig, N. W., Delgado-Friedrichs, O., O'Keeffe, M. and Yaghi,O. M., Reticular Chemistry: Occurrence and Taxonomy of Nets and Grammar for the Design of Frameworks,” Acc. Chem. Res.,38, 176-182(2005).
10. O'Keeffe, M., Eddaoudi, M., Li, H., Reineke, T. M. and Yaghi,O. M., “Frameworks for Extended Solids: Geometrical Design Principles,” J. Solid State Chem., 152, 3-20(2000).
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12. Rosseinsky, M., “Recent Developments in Metal–organic Framework Chemistry: Design, Discovery, Permanent Porosity and Flexibility,” Microporous Mesoporous Mater., 73, 15-30(2004).
13. Mori, W., Takamizawa, S., Kato, C. N., Ohmura, T. and Sato, T.,“Molecular-level Design of Efficient Microporous Materials Containing Metal Carboxylates: Inclusion Complex Formation with Organic Polymer, Gas-occlusion Properties, and Catalytic Activities for Hydrogenation of Olefins,” Microporous Mesoporous Mater.,73, 31-46(2004).
14. Sudik, A. C., Millward, A. R., Ockwig, N. W., Côté, A. P., Kim,J., Yaghi, O. M., Design, Synthesis, Structure, and Gas (N2, Ar,CO2, CH4, and H2) Sorption Properties of Porous Metal-Organic Tetrahedral and Heterocuboidal Polyhedra,” J. Am. Chem. Soc.,127, 7110-7118(2005).
15. Snurr, R., Hupp, J. and Nguyen, S. B., “Prospects for Nanoporous Metal-organic Materials in Advanced Separations Processes,”AIChE J., 50, 1090-1095(2004).
16. Rowsell, J. L. C. and Yaghi, O. M., “Strategies for Hydrogen Storage in Metal-organic Frameworks,” Angew. Chem. Int. Ed., 44,4670-4679(2005).
17. Millward, A. R. and Yaghi, O. M., “Metal−Organic Frameworks with Exceptionally High Capacity for Storage of Carbon Dioxide at Room Temperature,” J. Am. Chem. Soc., 127, 17998-17999(2005).
18. Bordiga, S., Lamberti, C., Ricchiardi, G., Regli, L., Bonino, F.,Damin, A., Lillerud, K. P., Bjorgen, M. and Zecchina, A., “Electronic and Vibrational Properties of a MOF-5 Metal–organic Framework: ZnO Quantum Dot Behaviour,” Chem. Commun.,2300-2301(2004).
19. Bisgaard, S., “Industrial Use of Statistically Designed Experiments:Case Study References and Some Historical Anecdotes,” Quality Eng., 4, 547-562(1992).
20. Sedghamiz, M. A., Raeissi, S, Attar, F., Salimi, M. and Mehrabi,K., “In-situ Transesterification of Residual Vegetable oil in Spent Bleaching Clay with Alkali Catalysts Using CCD-RSM Design of Experiment,” Fuel, 237, 515-521(2019).
21. Seki, Y., Seyhan, S. and Yurdakoc, M., “Removal of Boron from Aqueous Solution by Adsorption on Al2O3 Based Materials Using
Full Factorial Design,” J. Hazard. Mater., 138, 60-66(2006).
22. Ilzarbe, L., Alvarez, M. J., Viles, E. and Tanco, M., “Practical Applications of Design of Experiments in the Field of Engineering: A Bibliographical Review,” Qual. Reliab. Engng. Int., 24,417-428(2008).
23. Lee, M. H. and Yoo, K. S., “Optimization of MOF-801 Synthesis Using Sequential Design of Experiments,” Appl. Chem. Eng., 32,621-626(2021).
