Articles & Issues
- Language
- English
- Conflict of Interest
- In relation to this article, we declare that there is no conflict of interest.
- Publication history
-
Received May 27, 2009
Accepted August 23, 2009
- This is an Open-Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/bync/3.0) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.
Copyright © KIChE. All rights reserved.
All issues
Mesoporous silica synthesis in sub- and supercritcal carbon dioxide
Division of Food Science and Biotechnology, Pukyong National University, Busan, Korea 1Center for Molecular and Materials Sciences, Sansom Institute,School of Pharmacy and Medical Sciences, University of South Australia, Adelaide, SA 5000, Australia
phillip.pendleton@unisa.edu.au
Korean Journal of Chemical Engineering, March 2010, 27(3), 983-990(8), 10.1007/s11814-010-0130-x
Download PDF
Abstract
Mesoporous silicas were synthesized from sodium silicate (Na2Si3O7) and tetraethylorthosilicate (TEOS) with Pluronic F127 (polyethylene oxide-polypropylene oxide-polyethylene oxide, EO106PO70EO106) triblock copolymer using sub- and supercritical carbon dioxide (SubCO2 and SCO2) respectively, as solvents. Templates were removed using liquid carbon dioxide (LCO2) and SCO2. The most efficient template removal was achieved by LCO2 - 92.7% (w/w), followed by LCO2 with ethanol entrainer - 85.6% (w/w), and by methanol - 78.8% (w/w). The best efficiency of template removal by SCO2 was 50.7%. Values of specific surface areas, ABET, were increased by 10% with the increase of an ageing time from 6 to 24 hours for Na2Si3O7-based silicas at aqueous synthesis conditions, whereas the use of SCO2 reduced this value by 19.4%. For TEOS-based silicas synthesized using SCO2, A(BET) values increased by 3.8 times. Application of SCO2 for synthesis of TEOS-based silicas resulted in higher mesopore volumes of 0.719 and 1.241 mL/g with an average mesopore width varying from 3.4 to 3.9 nm. Although Na2Si3O7-based silicas have almost similar mesopore width range, their mesopore volumes were 7 times less than those for TEOS-based silicas. Formation of mesopores in Na2Si3O7- and TEOS-based silicas was at the expense of micropores when synthesized in SCO2.
Keywords
References
Palmqvist AEC, Curr. Opin. Colloid Interface Sci., 8, 145 (2003)
Zhao D, Huo Q, Feng J, Chmelka BF, Stucky GD, J. Am. Chem. Soc., 120(24), 6024 (1998)
Hanrahan JP, Copley MP, Spalding Trevor R, Holmes JD, Steytler DC, Amenitsch H, Steinhart M, Morris MA, J. Non-Cryst.Solids., 353, 4823 (2007)
Fulvio RF, Pikus S, Jaroniec M, JMCh, 15, 5049 (2005)
van Grieken R, Calleja G, Stucky GD, Melero JA, Garcia RA, Iglesias J, Langmuir, 19(9), 3966 (2003)
Huo QS, Feng JL, Schuth F, Stucky GD, Chemistry of Materials., 9, 14 (1997)
Lin CL, Pang YS, Chao MC, Chen BC, Lin HP, Tang CY, Lin CY, JPCS., 69, 415 (2008)
Chao MC, Chang CH, Lin HP, Tang CY, Lin CY, J. Mater. Sci., 44(24), 6453 (2009)
Wan Y, Zhao DY, Chem. Rev., 107(7), 2821 (2007)
Kim TW, Ryoo R, Kruk M, Gierszal KP, Jaroniec M, Kamiya S, Terasaki O, J. Phys. Chem. B, 108(31), 11480 (2004)
Cooper AI, Adv. Mater., 13(14), 1111 (2001)
Hanrahan JP, Copley MP, Ryan KM, Spalding TR, Morris MA, Holmes JD, Chem. Mater., 16, 424 (2004)
McHugh MA, Krukonis VJ, Supercritical fluid extraction (principles and practice); chemical reaction in supercritical fluids,2nd edition, Butterworth-Heinemann, Boston (1994)
Wakayama H, Goto Y, Fukushima Y, Physical Chemistry Chemical Physics., 5, 3784 (2003)
Tsoncheva T, Rosenholm J, Linden M, Ivanova L, Minchev C, Appl. Catal. A: Gen., 318, 234 (2007)
Kawi S, Lai MW, AIChE J., 48(7), 1572 (2002)
Badalyan A, Pendleton P, Wu H, Rev. Sci. Instrum., 72(7), 3038 (2001)
Badalyan A, Pendleton P, Langmuir, 19(19), 7919 (2003)
Gregg SJ, Sing KSW, Adsorption, surface area and porosity, Academic Press, London (1982)
Badalyan A, Pendleton P, J. Colloid Interface Sci., 326(1), 1 (2008)
Rouquerol F, Rouquerol J, Sing KSW, Adsorption by powders and porous solids, Academic Press, Sydney (1999)
Pure Appl. Chem., IUPAC, 66, 1739 (1994)
Saito A, Foley HC, AIChE J., 37, 429 (1991)
Lasaga AC, Cygan RT, AmMin., 67, 328 (1982)
Kim HY, Sofo JO, Velegol D, Cole, Milton W, Mukhopadhyay G, PhRvA., 72, 053201 (2005)
CRC handbook of chemistry and physics, 85th Edition, CRC Press (2004)
Barrett EP, Joyner LG, Halenda PP, J. American Chem. Soc., 73, 373 (1951)
Span R, Wagner W, JPCRD., 25, 1509 (1996)
Sato Y, Takikawa T, Yamane M, Takishima S, Masuoka H, Fluid Phase Equilib., 194-197, 847 (2002)
Pure Appl. Chem., IUPAC, 57, 603 (1985)
Kooyman PJ, Verhoef MJ, Prouzet E, Stud. Surf. Sci. Catal., (Nanoporous Materials II, Proceedings of the Conference on Access in Nanoporous Materials, 2000), 129, 535 (2000)
Ryoo R, Ko CH, Kruk M, Antochshuk V, Jaroniec M, J. Phys. Chem. B, 104(48), 11465 (2000)
Gobin OC, Wan Y, Zhao D, Kleitz F, Kaliaguine S, J. Phys.Chem. C., 111, 3053 (2007)
Arai Y, Sako T, Takebayashi Y, Supercritical fluids: Transport properties of supercritical fluids, Springer-Verlag, New York (2001)
Chun BS, Wilkinson GT, Ind. Eng. Chem. Res., 34(12), 4371 (1995)
Galarneau A, Cambon H, Di Renzo F, Ryoo R, Choi M, Fajula F, New Journal of Chemistry., 27, 73 (2003)
Bagshaw SA, Prouzet E, Pinnavaia TJ, Science., 269, 1243 (1995)
Kim SS, Pauly TR, Pinnavaia TJ, ChCom., 10, 835 (2000)
Zhao D, Huo Q, Feng J, Chmelka BF, Stucky GD, J. Am. Chem. Soc., 120(24), 6024 (1998)
Hanrahan JP, Copley MP, Spalding Trevor R, Holmes JD, Steytler DC, Amenitsch H, Steinhart M, Morris MA, J. Non-Cryst.Solids., 353, 4823 (2007)
Fulvio RF, Pikus S, Jaroniec M, JMCh, 15, 5049 (2005)
van Grieken R, Calleja G, Stucky GD, Melero JA, Garcia RA, Iglesias J, Langmuir, 19(9), 3966 (2003)
Huo QS, Feng JL, Schuth F, Stucky GD, Chemistry of Materials., 9, 14 (1997)
Lin CL, Pang YS, Chao MC, Chen BC, Lin HP, Tang CY, Lin CY, JPCS., 69, 415 (2008)
Chao MC, Chang CH, Lin HP, Tang CY, Lin CY, J. Mater. Sci., 44(24), 6453 (2009)
Wan Y, Zhao DY, Chem. Rev., 107(7), 2821 (2007)
Kim TW, Ryoo R, Kruk M, Gierszal KP, Jaroniec M, Kamiya S, Terasaki O, J. Phys. Chem. B, 108(31), 11480 (2004)
Cooper AI, Adv. Mater., 13(14), 1111 (2001)
Hanrahan JP, Copley MP, Ryan KM, Spalding TR, Morris MA, Holmes JD, Chem. Mater., 16, 424 (2004)
McHugh MA, Krukonis VJ, Supercritical fluid extraction (principles and practice); chemical reaction in supercritical fluids,2nd edition, Butterworth-Heinemann, Boston (1994)
Wakayama H, Goto Y, Fukushima Y, Physical Chemistry Chemical Physics., 5, 3784 (2003)
Tsoncheva T, Rosenholm J, Linden M, Ivanova L, Minchev C, Appl. Catal. A: Gen., 318, 234 (2007)
Kawi S, Lai MW, AIChE J., 48(7), 1572 (2002)
Badalyan A, Pendleton P, Wu H, Rev. Sci. Instrum., 72(7), 3038 (2001)
Badalyan A, Pendleton P, Langmuir, 19(19), 7919 (2003)
Gregg SJ, Sing KSW, Adsorption, surface area and porosity, Academic Press, London (1982)
Badalyan A, Pendleton P, J. Colloid Interface Sci., 326(1), 1 (2008)
Rouquerol F, Rouquerol J, Sing KSW, Adsorption by powders and porous solids, Academic Press, Sydney (1999)
Pure Appl. Chem., IUPAC, 66, 1739 (1994)
Saito A, Foley HC, AIChE J., 37, 429 (1991)
Lasaga AC, Cygan RT, AmMin., 67, 328 (1982)
Kim HY, Sofo JO, Velegol D, Cole, Milton W, Mukhopadhyay G, PhRvA., 72, 053201 (2005)
CRC handbook of chemistry and physics, 85th Edition, CRC Press (2004)
Barrett EP, Joyner LG, Halenda PP, J. American Chem. Soc., 73, 373 (1951)
Span R, Wagner W, JPCRD., 25, 1509 (1996)
Sato Y, Takikawa T, Yamane M, Takishima S, Masuoka H, Fluid Phase Equilib., 194-197, 847 (2002)
Pure Appl. Chem., IUPAC, 57, 603 (1985)
Kooyman PJ, Verhoef MJ, Prouzet E, Stud. Surf. Sci. Catal., (Nanoporous Materials II, Proceedings of the Conference on Access in Nanoporous Materials, 2000), 129, 535 (2000)
Ryoo R, Ko CH, Kruk M, Antochshuk V, Jaroniec M, J. Phys. Chem. B, 104(48), 11465 (2000)
Gobin OC, Wan Y, Zhao D, Kleitz F, Kaliaguine S, J. Phys.Chem. C., 111, 3053 (2007)
Arai Y, Sako T, Takebayashi Y, Supercritical fluids: Transport properties of supercritical fluids, Springer-Verlag, New York (2001)
Chun BS, Wilkinson GT, Ind. Eng. Chem. Res., 34(12), 4371 (1995)
Galarneau A, Cambon H, Di Renzo F, Ryoo R, Choi M, Fajula F, New Journal of Chemistry., 27, 73 (2003)
Bagshaw SA, Prouzet E, Pinnavaia TJ, Science., 269, 1243 (1995)
Kim SS, Pauly TR, Pinnavaia TJ, ChCom., 10, 835 (2000)