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Porous Texture and Surface Character of Dehydroxylated and Rehydroxylated MCM-41 Mesoporous Silicas—Analysis of Adsorption Isotherms of Nitrogen Gas and Water Vapor

✍ Scribed by Hiromitu Naono; Masako Hakuman; Takashi Tanaka; Nobuki Tamura; Kazuyuki Nakai


Publisher
Elsevier Science
Year
2000
Tongue
English
Weight
209 KB
Volume
225
Category
Article
ISSN
0021-9797

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✦ Synopsis


Four samples of MCM-41 mesoporous silicas whose average pore diameters are 2.4, 2.8, 3.2, and 3.6 nm were prepared using sodium orthosilicate and cationic surfactants of [CH(3)(CH(2))(n)N(CH(3))(3)]X (n=11, 13, 15, 17). These four samples were calcined at 1123 K in vacuo to obtain the dehydroxylated samples, which were further rehydroxylated at 298 K to obtain the rehydroxylated samples. The adsorption isotherms of nitrogen gas (77 K) for the 12 MCM-41 mesoporous silicas are of Type IVc, giving no adsorption hysteresis. On the other hand, the first adsorption isotherms of water vapor (298 K) for the dehydroxylated MCM-41 samples are quite different from those of nitrogen gas, giving the remarkable adsorption hysteresis. The second water isotherms for the rehydroxylated MCM-41 samples are of Type IV, showing slight hysteresis. Using the nitrogen isotherms, the relation between the pore size and carbon chain length of the surfactant has been determined, and the effect of dehydroxylation and rehydroxylation on the porous texture has been examined. Using the first and second water isotherms, the adsorption model of physisorbed waters adsorbed on the surface silanol groups has been proposed. From the pore size distribution curves of nitrogen and water, the presence of constrictions in the cylindrical pores has been predicted. Copyright 2000 Academic Press.


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The adsorption isotherms of N 2 gas at 77 K and CCl 4 vapor at 283.1 5 , 298.1 5 , and 308.1 5 K were measured for six samples of the mesoporous silicas having uniform cylindrical pores (MCM-41). The pore radii of the six samples (r p ), which were evaluated from the α s plots of the N 2 isotherms,