Isothermal template removal from MCM-41 in hydrogen flow

被引:15
作者
Goworek, Jacek [1 ]
Kierys, Agnieszka [1 ]
Kusak, Ryszard [1 ]
机构
[1] Marie Curie Sklodowska Univ, Fac Chem, Dept Adsorpt, PL-20031 Lublin, Poland
关键词
MCM-41; silica; template removal; GC-MS; CHN; NMR; adsorption;
D O I
10.1016/j.micromeso.2006.09.011
中图分类号
O69 [应用化学];
学科分类号
081704 ;
摘要
Thermal evacuation of template surfactant from MCM-41 in hydrogen atmosphere was investigated. Micelle templated silica was prepared using hexadecyltrimethylammonium bromide. The mechanism of template removal appears to be completely different in hydrogen as compared to calcination in air. It seems that moderate heating of as-synthesized MCM-41 (up to about 250 degrees C) in hydrogen stream for about 15 h is effective and simple method of template removal leaving no pure carbon residues on silica surface. Adsorption properties of partially evacuated MCM-41 samples were tested using gas chromatography. Products of template degradation were analyzed using GC-MS technique. The main products of template degradation at 250 degrees C in hydrogen flow are hexadecene and hexadecane-N,N-dimethylamine. Concentration of surface silanols for MCM-41 calcined and thermally treated in hydrogen flow was investigated by NMR technique. (C) 2006 Elsevier Inc. All rights reserved.
引用
收藏
页码:242 / 248
页数:7
相关论文
共 22 条
[1]   THE DETERMINATION OF PORE VOLUME AND AREA DISTRIBUTIONS IN POROUS SUBSTANCES .1. COMPUTATIONS FROM NITROGEN ISOTHERMS [J].
BARRETT, EP ;
JOYNER, LG ;
HALENDA, PP .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1951, 73 (01) :373-380
[2]  
BEK JS, 1992, J AM CHEM SOC, V114, P10834
[3]   Postsynthesis hydrothermal restructuring of M41S mesoporous molecular sieves in water [J].
Chen, LY ;
Horiuchi, T ;
Mori, T ;
Maeda, K .
JOURNAL OF PHYSICAL CHEMISTRY B, 1999, 103 (08) :1216-1222
[4]   Adsorption of aromatic hydrocarbons on highly siliceous MCM-41 [J].
Choudhary, VR ;
Mantri, K .
LANGMUIR, 2000, 16 (17) :7031-7037
[5]   Enhanced n-hexane diffusion in partially filled MCM-41 of different surface hydrophobicity probed by NMR [J].
Courivaud, F ;
Hansen, EW ;
Kolboe, S ;
Karlsson, A ;
Stöcker, M .
MICROPOROUS AND MESOPOROUS MATERIALS, 2000, 37 (1-2) :223-232
[6]   Determination of the hydroxyl group content in Silica by thermogravimetry and a comparison with 1H MAS NMR results [J].
Ek, S ;
Root, A ;
Peussa, M ;
Niinistö, L .
THERMOCHIMICA ACTA, 2001, 379 (1-2) :201-212
[7]  
GRUN M, 1997, CHARACTERIZATION POR, V4, P81
[8]   Characterization of the acid sites in MCM-41-type materials by spectroscopic and catalytic techniques [J].
Hunger, M ;
Schenk, U ;
Breuninger, M ;
Gläser, R ;
Weitkamp, J .
MICROPOROUS AND MESOPOROUS MATERIALS, 1999, 27 (2-3) :261-271
[9]   Calcination behavior of different surfactant-templated mesostructured silica materials [J].
Kleitz, F ;
Schmidt, W ;
Schüth, F .
MICROPOROUS AND MESOPOROUS MATERIALS, 2003, 65 (01) :1-29
[10]   Evolution of mesoporous materials during the calcination process:: structural and chemical behavior [J].
Kleitz, F ;
Schmidt, W ;
Schüth, F .
MICROPOROUS AND MESOPOROUS MATERIALS, 2001, 44 :95-109