Tailoring Particle Size and Agglomeration State of Mesoporous MCM-48 via Optimisation of Sol-gel Silica Process
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Abstract
Mobil Composition of Matter no. 48 (MCM-48) is a promising inorganic particle due to its unique crystal structure and 3-dimensional porous network. Incorporating a discrete amount of nanosized MCM-48 for material development would give significant impact to the material’s performance and mechanical robustness. Thus far, the synthesis of MCM-48 in the nanoscale regime has been achieved via chemical modification techniques. However, they are often not reproducible due to limited understanding of surfactant behaviour. On the other hand, physical modification technique is more stable, thereby can reduce the possibility of producing other undesired mesophase. Nevertheless, this technique has not been adapted for nanosized MCM-48 synthesis. In this work, the physical modification technique was adapted to tailor MCM-48 particle size by varying stirring speed (i.e., 1000 rpm, 3000 rpm and 5000 rpm) and using different types of washing medium. Particle size distribution (PSD) studies showed mean particle size of 250 ± 50 nm. XRD analysis displayed several crystalline peaks indexed to cubic crystal mesophase. Transmission electron microscopy (TEM) and Brunauer-Emmett Teller (BET) analyses also showed a unique 3D cubic interconnecting porous network with specific surface area of 1030 m2 g–1. It was revealed that the degree of agglomeration increased as relative polarity of alcohol increased, CH3OH > CH3CH2OH. Therefore, particle size and agglomeration state of MCM-48 can be tailored by varying the physical modification techniques while maintaining its intrinsic pore morphology.
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References
Halamová, D. et al. (2010). Naproxen drug delivery using periodic mesoporous silica SBA-15. Appl. Surf. Sci., 256, 6489–6494, https://doi.org/doi_10.1016/j.apsusc.2010.04.044.
Maheswari, R. et al. (2014). Synthesis, characterization, and epoxidation activity of tungsten-incorporated SBA-16 (W-SBA-16). Ind. Eng. Chem. Res., 53, 18833–18839, https://doi.org/10.1021/ie501784c.
Kishor, R. & Ghoshal, A. K. (2015). APTES grafted ordered mesoporous silica KIT-6 for CO2 adsorption. Chem. Eng. J., 262, 882–890, https://doi.org/10.1016/j.cej.2014.10.039.
Coasne, B. et al. (2006). Gas adsorption in mesoporous micelle-templated silicas: MCM-41, MCM-48, and SBA-15. Langmuir, 22, 11097–11105, https://doi.org/10.1021/la061728h.
Changbum, J. et al. (2009) Syntheses of high quality KIT-6 and SBA-15 mesoporous silicas using low-cost water glass, through rapid quenching of silicate structure in acidic solution. Microp. Mesop. Mater., 124, 45–51, https://doi.org/10.1016/J.MICROMESO.2009.04.037.
Roth, W. J. (2009). Facile synthesis of the cubic mesoporous material MCM-48: Detailed study of accompanying phase transformations. Adsorp., 15, 221–226. https://doi.org/10.1007/s10450-009-9161-1.
Monnier, A. et al. (1993). Cooperative formation of inorganic-organic interfaces in the synthesis of silicate mesostructures. Sci., 80(261), 1299–1303, https://doi.org/10.1126/science.261.5126.1299.
Vartuli, J. et al. (1998). The synthesis and properties of M41S and related mesoporous materials. Synth. (Stuttg)., 1, 97–119, https://doi.org/10.1007/3-540-69615-6_4.
Firouzi, A. et al. (1997). Alkaline lyotropic silicate-surfactant liquid crystals. J. Am. Chem. Soc., 119, 3596–3610, https://doi.org/10.1021/ja963007i.
Narayan, K. R. et al. (1996). Template-based approaches to the preparation of amorphous, nanoporous silicas. Chem. Mater., 8(8), 1682–1701, https://doi.org/10.1021/CM960138.
Qisheng, H., Margolese, D. I. & Stucky, G. D. (1996). Surfactant control of phases in the synthesis of mesoporous silica-based materials. Chem. Mater., 8(5), 1147–1160, https://doi.org/10.1021/CM960137H.
Kumar, D. et al. (2001). MCM-41, MCM-48 and related mesoporous adsorbents: Their synthesis and characterisation. Coll. Surf. A Physicochem. Eng. Asp., 187–188, 109–116, https://doi.org/10.1016/S0927-7757(01)00638-0.
Petitto, C. et al. (2005). Synthesis of discrete micrometer-sized spherical particles of MCM-48. Chem. Mater., 17, 2120–2130, https://doi.org/10.1021/cm050068j.
Díaz, I., Alfredsson, V. & Sakamoto, Y. (2006). Transmission electron microscopy in formation and growth of ordered mesoporous materials. Curr. Opin. Coll. Interf. Sci., 11, 302–307, https://doi.org/doi_10.1016/j.cocis.2006.09.007.
Rahman, I. A. et al. (2007). An optimized sol-gel synthesis of stable primary equivalent silica particles. Coll. Surf. A Physicochem. Eng. Asp., 294, 102–110, https://doi.org/10.1016/j.colsurfa.2006.08.001.
Schumacher, K., Grün, M. & Unger, K. (1999). Novel synthesis of spherical MCM-48. Microp. Mesop. Mater., 27, 201–206, https://doi.org/10.1016/s1387-1811(98)00254-6.
Jomekian, A. et al. (2011). Fabrication or preparation and characterization of new modified MCM-41/PSf nanocomposite membrane coated by PDMS. Sep. Purif. Technol., 80, 556–565, https://doi.org/10.1016/J.SEPPUR.2011.06.011.
Meléndez-Ortiz, H. I. et al. (2014). Functionalization with amine-containing organosilane of mesoporous silica MCM-41 and MCM-48 obtained at room temperature. Ceram. Int., 40(7), 9701–9707, https://doi.org/10.1016/j.ceramint.2014.02.051.
Meléndez-Ortiz, H. I. et al. (2014). Influence of the reaction conditions on the thermal stability of mesoporous MCM-48 silica obtained at room temperature. Ceram. Int., 40, 4155–4161, https://doi.org/10.1016/j.ceramint.2013.08.072.
Jomekian, A. et al. (2011). Gas transport behavior of DMDCS modified MCM-48/ polysulfone mixed matrix membrane coated by PDMS. Kor. J. Chem. Eng., 28, 2069–2075, https://doi.org/10.1007/s11814-011-0075-8.
Kim, T.-W., Chung, P.-W. & Lin, V. S.-Y. (2010). Facile synthesis of monodisperse spherical MCM-48 mesoporous silica nanoparticles with controlled particle size. Chem. Mater., 22, 5093–5104, https://doi.org/doi_10.1021/cm1017344.
Wei, F. Y. et al. (2010). Synthesis of mesoporous MCM-48 using fumed silica and mixed surfactants. Microp. Mesop. Mater., 131, 224–229, https://doi.org/10.1016/j.micromeso.2009.12.027.
Banerjee, S. et al. (2010). Pd-MCM-48: A novel recyclable heterogeneous catalyst for chemo- and regioselective hydrogenation of olefins and coupling reactions. Org. Biomol. Chem., 8, 4316, https://doi.org/doi_ 10.1039/c0ob00183j.
Boote, B., Subramanian, H. & Ranjit, K. T. (2007). Rapid and facile synthesis of siliceous MCM-48 mesoporous materials. Chem. Commun., 4543–4545. https://doi.org/10.1039/b706633c.
Tae, W. K. et al. (2004). Tailoring the pore structure of SBA-16 silica molecular sieve through the use of copolymer blends and control of synthesis temperature and time. J. Phys. Chem. B, 108(31), 11480–11489, https://doi.org/10.1021/jp048582k.
Chen, P.-K. et al. (2013). New synthesis of MCM-48 nanospheres and facile replication to mesoporous platinum nanospheres as highly active electrocatalysts for the oxygen reduction reaction. Chem. Mater., 25, 4269–4277, https://doi.org/10.1021/cm402349f.
Díaz, I., Pérez-Pariente, J. & Terasaki, O. (2004). Structural study by transmission and scanning electron microscopy of the time-dependent structural change in M41S mesoporous silica (MCM-41 to MCM-48, and MCM-50). J. Mater. Chem., 14, 48–53, https://doi.org/10.1039/B310281E.
Zhai, S. R. et al. (2002). The synthesis of mesoporous molecular sieve MCM-48 using two surfactants as co-template. Acta Phys. Chim. Sin., 18, 911–915, https://doi.org/10.3866/PKU.WHXB20021009.
Zhao, W. et al. (2010). Synthesis of high quality MCM-48 with binary cationic-nonionic surfactants. Langmuir, 26, 6982–6988, https://doi.org/10.1021/la9042155.
Kaskel, S. (2008). Characterisation of porous solids VIII. Paper presented at the Proceedings of the 8th International Symposium on the Characterisation of Porous Solids, 10–13 June, Edinburgh.
Rouquerol, J. et al. (1994). Recommendations for the characterization of porous solids (technical report). Pure Appl. Chem., 66, 1739–1758, https://doi.org/10.1351/pac199466081739
Alfredsson, V. & Anderson, M. W. (1996). Structure of MCM-48 revealed by transmission electron microscopy. Chem. Mater., 8, 1141–1146, https://doi.org/10.1021/cm950568k.
Schumacher, K. et al. (2000). Characterization of MCM-48 Materials. Langmuir, 16, 4648–4654, https://doi.org/10.1021/la991595i.
Sang, W. Y. & Ching, O. P. (2017). Tailoring MCM-41 mesoporous silica particles through modified sol-gel process for gas separation. Paper presented at the in AIP Conference Proceedings 1891, 3–5 April, Kedah, Malaysia, https://doi.org/10.1063/1.5005480.