SYNTHESIS AND CHARACTERIZATION OF MCM-41 AND METAL-SUPPORTED MCM-41 MATERIALS USING DIFFERENT METHODS

Abstract

One of the known groups of mesoporous materials is MCM-41 that has been applied as catalyst for various chemical reactions. In the content of this study, using cetylytrimethylammonium bromide (CTAB) as surfactant, sodium silicate and tetraethylortosilicate (TEOS) as silica source mesoporous materials MCM-41 was synthesized by hydrothermal synthesis method and sonochemical synthesis method. The obtained results showed that MCM-41 synthesized by the sonochemical method had higher specific surface area and pore volume than those synthesized by the hydrothermal method. Also, the effects of silica source on the distribution of products were studied and sodium silicate was found to be more suitable for the synthesis of MCM-41. Based on determinated optimum conditions, MCM-41 supported Al, Co and Fe having different ratios of metal (Metal/Si: ratio 0.05, 0.1 and 0.2) was synthesized. It was observed that metal dispersion on MCM-41 was homogenous for all samples and its particles sizes were between 10 nm to 30 nm. Synthesized mesoporous materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersion spectroscopy (EDS) and Brunauer Emmett Teller (BET) surface area methods.

Keywords

• MCM-41
• mesoporous materials
• hydrothermal method
• sonochemical method
• synthesis
• characterization

References

1. Jabariyan, S., Zanjanchi, M. A., A simple and fast sonication procedure to remove surfactant templates from mesoporous MCM-41, Ultrasonics Sonochemistry, 19 (2012), 1087-1093.
2. Øye, G., Glomm, W. R., Vrålstad, T., Volden, S., Magnusson, H., Stöcker, M., Sjöblom, J., Synthesis, functionalization and characterization of mesoporous materials and sol-gel glasses for application in catalysis, adsorption and photonics, Advances in Colloid and Interface Science, 123 (2006), 17-32.
3. Jentys, A., Pham, N. H., Vinek, H., Englisch, M., Lercher, J. A., Synthesis and characterization of mesoporic materials containing highly dispersed cobalt, Microporous Materials, 68 (1996), 13-17.
4. Beck, J. S., Vartuli, J. C., Roth, W. J., Leonowicz, M. E., Kresge, C. T., Schmitt, K. D., Chu, C. T. W., Olson, D. H., Sheppard, E. W., McCullen, S. B., Higgins, J. B., Schlenker, J. L., A new family of mesoporous molecular sieves prepared with liquid crystal templates, Journal of the American Chemical Society, 114 (1992),10834-10843.
5. Nejabat, G. R., Nekoomanesh, M., Arabi, H., Emami, M., Aghaei-Nieat, M., Preparation of polyethylene nano-fibres using rod-like MCM-41/TiCl4/MgCl2/THF Bi-supported Ziegler-natta catalytic system, Iranian Polymer Journal, 19 (2010), 79-87.
6. Huang, R. H., Liu, J., Li, L. S., Zhang, Q. Y., Zeng, L. X., Lu, P., Fe/MCM-41 as a promising heterogeneous catalyst for ozonation of p-chlorobenzoic acid in aqueous solution, Chinese Chemical Letters, 22 (2011), 683-686.
7. Gucbilmez, Y., Dogu, T., Balci, S., Vanadium incorporated high surface area MCM-41 catalysts, Catalysis Today, 100 (2005), 473-477.
8. Gaydhankar, T. R., Samuel, V., Jha, R. K., Kumar, R., Joshi, P. N., Room temperature synthesis of Si-MCM-41 using polymeric version of ethyl silicate as a source of silica, Materials Research Bulletin, 42 (2007),1473-1484.

9. Voegtlin, A. C., Matijasic, A., Patarin, J., Sauerland, C., Grillet, Y., Huve, L., Room-temperature synthesis of silicate mesoporous MCM-41-type materials: influence of synthesis pH on the porosity of the materials obtained, Microporous Materials, 10 (1997), 137-147.
10. Kruk, M., Jaronice, M., Sayari, A., Structure and surface properties of siliceous and titanium-modified HMS molecular sieves, Microporous and Mesoporous Materials, 35 (2000), 545-553.
11. Aquino, J. M. F. B., Souza, C. D. R., Aroujo, A. S., Synthesis and characterization of sulfate-supported MCM-41 material, International Journal of Inorganic Materials, 3(2001), 467-470.
12. Tai, X. M., Wang, H. X., Shi, X. Q., A novel method for the synthesis of mesoporous molecular sieve MCM-41, Chinese Chemical Letter, 16 (2005), 843-845.
13. Zanjanchi, M. A., Asgari, S., Incorporotion of aluminum into the framework of mesoporous MCM-41: the contribution of diffuse reflectance spectroscopy, Solid State Ionics, 171 (2004), 277-282.
14. Melo, R. A. A, Giottoa, M. V., Rochab, J., Ernesto, A. González, U., MCM-41 Ordered mesoporous molecular sieve synthesis and characterization, Materials Research, 2 (1999), 173-179.
15. Suslick, K. S., Interparticle collisions driven by ultrasound, Science, 247 (1990), 1437-1445.
16. Horòáèek, M., Hudec, P., Smiešková, A., Syntesis and characterization of mesoporous molecular sieves, Chemical Papers, 63 (2009), 689-697.
17. Sun, Z., Wang, L., Liu, P., Sun, B., Jiang, D., Xiao, F., Synthesis and catalytic activity of Cu-incorporated MCM-41 with spheres-within-a-sphere hollow structure, Chinese Journal of Chemistry, 24(2006), 1653-1656.
18. Eimer, G. A., Pierella, L. B., Monti, G. A., Anunziata, O. A., Synthesis and characterization of Al-MCM-41 and Al-MCM-48 mesoporous materials, Catalysis Letters, 78 (2002), 65-75.
19. Huang, R. H., Liu, J, Li, L. S., Zhang, Q. Y., Zeng, L. X., Lu, P., Fe/MCM-41 as a promising heterogeneous catalyst for ozonation of p-chlorobenzoic acid in aqueous solution, Chinese Chemical Letters, 22 (2011), 683-686.
20. Lemus, I. A., Gomez, Y. V., Elguézabal, A. A., Contreras, L. A., Metal nanoparticles supported on Al-MCM-41 via in situ aqueous synthesis, Journal of Nanomaterials, 2010 (2010), 1-8.
21. Gedikli, Ü., Mısırlıoğlu, Z., Bozkurt P. A., Canel, M., Synthesis of MCM-41 by hydrothermal and sonochemical methods and characterization, Journal of the Turkish Chemical Society, Section A: Chemistry, 2 (2015), 54-58.
22. Li, Q., Brown, S. E., Broadbelt, L. J., Zheng, J. G., Wu, N. Q., Synthesis and characterization of MCM-41 supported Ba2SiO4 base catalyst, Microporous and Mesoporous Materials, 59 (2003), 105-111.
23. Lensveld, D. J., Mesu, J. G., Dillen, A. J., Jong, K. P., Synthesis and characterization of MCM-41 supported nickel oxide catalyst, Microporous and Mesoporous Materials, 44 (2001), 401-407.
24. Hui, K. S., Chao, C. Y. H., Synthesis of MCM-41 from coal fly ash by a green approach: Influence of synthesis pH, Journal of Hazardous Materials B, 137 (2006), 1135-1148.
25. Fu, L., Zhang, H., Preparation, characterization and luminescent properties of MCM-41 type materials impregnated with rare earth complex, Journal of Materials Science and Technology, 17 (2001), 293-298.
26. Somani, R. S., Textural and structural properties of mesoporous silica synthesized under refluxing conditions, Journal of Porous Materials, 12 (2005), 87-94.
27. Laha, S. C., Mukherjee, P., Kumar, R., Synthesis and characterization of surface-modified and organic-functionalized MCM-41 type ordered mesoporous materials, Bulletin of Materials Science, 22 (1999), 623-626.
28. Liu, D., Quek, X. Y., Cheo, W. N. E., Lau, R., Borgna, A., Yang, Y., MCM-41 supported nickel-based bimetallic catalysts with superior stability during carbon dioxide reforming of methane: effect of strong metal-support interaction, Journal of Catalysis, 266 (2009), 380-390.
29. Blin, J. L., Otjacques, C., Herrier, G, Su, B. L., Kinetic study of MCM-41 synthesis, International Journal of Inorganic Materials, 3 (2001) 75-86.
30. Yu, J., Shi, J. L., Wang, L. Z., Ruan, M. L., Yan, D. S., Preparation of high thermal stability MCM-41 in the low surfactant/silicon molar ration synthesis systems, Materials Letters, 48 (2001), 112-116.