EFFECT OF AGING TIME TOWARD CRYSTALLINITY OF PRODUCTS IN SYNTHESIS OF MESOPOROUS SILICATES MCM-41

https://doi.org/10.22146/ijc.21435

Suyanta Suyanta(1*), Narsito Narsito(2), Endang Tri Wahyuni(3), Triyono Triyono(4), Sutarno Sutarno(5)

(1) Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Gadjah Mada, Sekip Utara, Kotak Pos 21 Bls Yogyakarta 55281
(2) Department of Chemistry, Faculty of Mathematics and Natural Sciences,Universitas Gadjah Mada, Jl. Sekip Utara, Pos Box: BLS 21, Yogyakarta 55281
(3) Department of Chemistry, Faculty of Mathematics and Natural Sciences,Universitas Gadjah Mada, Jl. Sekip Utara, Pos Box: BLS 21, Yogyakarta 55281
(4) Department of Chemistry, Faculty of Mathematics and Natural Sciences,Universitas Gadjah Mada, Jl. Sekip Utara, Pos Box: BLS 21, Yogyakarta 55281
(5) Department of Chemistry, Faculty of Mathematics and Natural Sciences,Universitas Gadjah Mada, Jl. Sekip Utara, Pos Box: BLS 21, Yogyakarta 55281
(*) Corresponding Author

Abstract


Researches about the effects of aging time toward crystallinity of products in the synthesis of mesoporous silicates MCM-41 have been done. MCM-41 was synthesized by hydrothermal treatment to the mixture of sodium silicate, sodium hydroxide, cetyltrimetylammoniumbromide (CTMAB) and aquadest in the molar ratio of 8Na2SiO3 : CTMAB : NaOH : 400H2O. Hydrothermal treatment was carried out at 110 °C in a teflon-lined stainless steel autoclave heated in the oven, with variation of aging time, i.e.: 4, 8, 12, 16, 24, 36, 48, and 72 h respectively. The solid phase were filtered, then washed with deionised water, and dried in the oven at 100 °C for 2 h. The surfactant CTMAB was removed by calcinations at 550 °C for 10 h with heating rate 2 °C/min. The as-synthesized and calcined powders were characterized by using FTIR spectroscopy and X-ray diffraction method. The relative crystallinity of products was evaluated based on the intensity of d100 peaks. The best product was characterized by using N2 physisorption method in order to determine the specific surface area, mean pore diameter, lattice parameter, and pore walls thickness. It was concluded that the relative crystallinity of the products was sensitively influenced by the aging time. The highest relative crystallinity was achieved when used 36 h of aging time in hydrothermal treatment. In this optimum condition the product has 946.607 m2g-1 of specific surface area, 3.357 nm of mean pore diameter, 4.533 nm of lattice parameter, and 1.176 nm of pore walls thickness.

Keywords


MCM-41; crystallinity; aging time

Full Text:

Full Text PDF


References

[1]   Kresge, C.T., Leonowicz, M.E., Roth, W.J., Vartuli, J.C., and Beck, J.S., 1992, Nature, 359, 710-712.

[2]   Monnier, A., Schüth, F., Huo, Q., Kumar, D., Margolese, D., Maxwell, R.S., Stucky, G.D., Krishnamurty, M., Petroff, P., Firouzi, A., Janicke, M., and Chmelka, B.F., 1993, Science, 261, 5126, 1299-1303.

[3]   Huo, Q., Margolese, D., Siesla, U., Feng, P., Gler, T.E., Sieger, P., Leon, R., Petroff, P., Schüth, F., and Stucky, G.D., 1994, Nature, 368, 317-321.

[4]   Huo, Q., Margolese, D.I., and Stucky, G.D., 1996, Chem. Mater., 8, 5, 1147-1160.

[5]   Yoshitake, H., Yokoi, T., and Tatsumi, T., 2002, Chem. Mater., 14, 11, 4603-4610.

[6]   Oshima, S., Perera, J.M., Northcott, K.A., Kokusen, H., Stevens, G.W., and Komatsu,Y., 2006, Sep. Sci. Technol., 41, 8, 1635–1643.

[7]   Bhattacharyya, K.G., Talukdar, A.K., Das, P., and Sivasanker, S., 2003, J. Mol. Catal. A: Chem., 197, 255-252.

[8]   Xin, H., Liu, J., Fan, F., Feng, Z., Jia, G., Yang, Q., and Li, C., 2008, Microporous Mesoporous Mater., 113, 1-3, 231–239.

[9]   Catana, R., Ferreira, J.M.S., Cabral, J.M.S., and Fernandes, P., 2005, Food Chem., 91, 3, 517–520.

[10] Curulli, A., Cusma, A., Kaciulis, S., Padeletti, G., Pandolfi, L., Valentini, F., and Vitocelli, M., 2006, Surf. Interface Anal., 38, 4, 478–481.

[11] Vallet-Regi M., Doadrio J.C., Doadrio A.L., Izquierdo-Barba, I., and Pérez-Pariente, J., 2004, Solid State Ionics, 172, 1-4, 435-439.

[12] Huang, S., Fan, Y., Cheng, Z., Kong, D., Yang, P., Quan, Z., Zhang, C., and Lin, J., 2009, J. Phys. Chem. C, 113, 5, 1775–1784.

[13] Dapurkar, S.E., Badamali, S.K., and Selvam P., 2001, Catal. Today, 68, 1-3, 63–68.

[14] Kruk, M.;,Jaroniec, M., and Sayari, A., 1999, J. Phys. Chem. B, 103, 4590-4598.

[15] Kim, J.M. and Ryoo, R., 1996, Bull. Korean Chem. Soc., 17, 1, 66–68.

[16] Mori, T., Kuroda, Y., Yoshikawa, Y., Nagao, M., and Kittaka, S., 2002, Langmuir, 18, 5, 1595–1603.

[17] Parfenov, V.A. and Kirik, S.D., 2003, Chemistry for Sustainable Development, 11, 735–740.

[18] Flanigen, E.M., Khatami, H., and Szymanski, H.A., 1971, Infrared Structural Studies of Zeolite Frameworks, In Flanigen, E.M., and Sand, L.B., eds., Molecular Sieve Zeolites., ACS Adv. Chem. Ser., 101, 290-227.

[19] Brinker, C.J., and Scherer, G.W., 1990, Sol-Gel Science; Academic Press: Boston, 908.

[20] Beck, J.S. and Vartuli, J.C., 1996, Curr. Opin. Solid State Mater. Sci., 1, 1, 76–87.

[21] Shen, S.C., and Kawi, S., 1999, J. Phys. Chem. B, 103, 42, 8870–8876.

[22] Zhao, X.S., Lu, G.Q.M., and Millar, G.J., 1996, Advances in mesoporous molecular sieve MCM 41, Ind. Eng. Chem. Res., 35, 7, 2075–2090.

[23] Selvam, P., Bhatia, S.K., and Sonwane, C.G., 2001, Ind. Eng. Chem. Res., 40, 15, 3237–3261.

[24] Gusev, V.Y., Feng, X., Bu, Z., Haller, G.L., and O’Brien, J.A., 1996, J. Phys. Chem., 100, 6, 1985–1988.

[25] Mohammed, A.B., 2005, Synthesis, Characterization and Activity of Al-MCM-41 Catalyst for Hydroxyalkylation of Epoxides, Thesis, Universiti Teknologi Malaysia, 52-53.



DOI: https://doi.org/10.22146/ijc.21435

Article Metrics

Abstract views : 369 | views : 382


Copyright (c) 2010 Indonesian Journal of Chemistry

Creative Commons License
This work is licensed under a Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.

 


Indonesian Journal of Chemisty (ISSN 1411-9420 / 2460-1578) - Chemistry Department, Universitas Gadjah Mada, Indonesia.

Web
Analytics View The Statistics of Indones. J. Chem.