Superbasic sites have been generated on the mesoporous silica materials for the first time, through a
new strategy to prepare the MgO-modified SBA-15 in one-pot synthesis and then to disperse KNO3,
possessing the good textural structure of the host and the high basic strength (H
-) of 27.0. The in situ
coated Mg species passivated the silanol groups on the surface of siliceous SBA-15 so that the
mesostructure of SBA-15 could be reserved after the composite was loaded with KNO3 and activated at
high temperature. Existence of the special protection layer of MgO on the surface of SBA-15 was also
beneficial for decomposition of KNO3 to form superbasic sites on the mesoporous silica. The influence
of coating amount of MgO on the protection of the textural properties of SBA-15 is examined and discussed
in terms of consuming surface silanol groups. Dispersion and decomposition of KNO3 on the MgO layer
is also explored. Other metal oxides such as CaO, ZnO, and Al2O3 are in situ coated on the surface of
SBA-15 through one-pot synthesis and their function of protecting SBA-15 is evaluated for comparison
with MgO.
Aluminum‐containing plugged mesoporous silica has been successfully prepared in an aqueous solution that contains triblock copolymer templates, nitrates, and silica sources but without using mineral acid. The acidity of the solution can be finely tuned from pH 1.4 to 2.8 according to the amount of the introduced aluminum species which ranged from an Al/Si molar ratio of 0.25/1 to 4.0/1. The aluminum nitrate additive in the starting mixture, along with the weak acidity produced by the nitrates, contributes to the formation of plugged hexagonal structures and the introduction of different amounts of aluminum species into the mesostructure. Characterization by X‐ray diffraction, transmission electron microscopy, and N2 sorption measurements show that the Al‐containing plugged silicas possess well‐ordered hexagonal mesostructures with high surface areas (700–860 m2 g–1), large pore volume (0.77–1.05 cm3 g–1) and, more importantly, combined micropores and/or small mesopores in the cylindrical channels. Inductively coupled plasma–atomic emission spectrometry results show that 0.7–3.0 wt % aluminum can be introduced into the final samples. 27Al MAS NMR results display that about 43–60% aluminum species are incorporated into the skeleton of the Al‐containing silicas and the amount of the framework aluminum increases as the initial added nitrates rises. Scanning electron microscopy images reveal that the directly synthesized Al‐containing plugged silica has a similar morphology to that of traditional SBA‐15. Furthermore, the Al‐containing plugged samples have excellent performances in the adsorption and the catalytic decomposition of isopropyl alcohol and nitrosamine. Finally, the direct synthesis method is used to produce plugged mesoporous silicas that contain other metals such as chromium and copper, and the resultant samples also show good catalytic activities.
Solid‐state grinding is a simple and effective method to include guest species into the channels of ordered mesoporous materials with a different degree of filling. After calcination, a monolayer or several monolayers of guest species can not only form highly dispersed oxide species and other surface species on the hosts whether the template is occluded in the channels or not, but the guest species can also fill the mesoporous channels in the host and thus lead to nanowires or nanoarrays. Solid‐state salt inclusion is faster and more convenient than other inclusion routes. The absence of a solvent not only saves the time otherwise needed for evaporation but also leads to a higher degree of filling through a simple inclusion step as the void space in the pores is not occupied by the solvent. Also, the lack of competitive adsorption of solvent molecules enhances the interaction between the guest species included and the silica wall, which facilitates the high dispersion of oxide species. However, host–guest interactions that are too strong may disturb the self‐crystallization of guest species in the mesopores leading to imperfect nanocasting of the mesostructure.
The adsorption and catalytic degradation of nitrosamines by zeolite A with cesium, potassium, sodium, or calcium cation was systemically studied in the research reported in this article. The results of instantaneous adsorption, temperature-programmed surface reaction, and in situ Fourier transform infrared spectroscopy measurements proved the adsorption of the bulky nitrosamines, N′-nitrosonornicotine (NNN) and Nnitrosopyrrolidine, on the zeolite A with a pore diameter of only 0.2-0.5 nm. Moreover, thermogravimetricmass spectrometry analysis revealed the different adsorption and degradation manners of NNN on various samples of zeolite A, which will be discussed in terms of electrostatic attraction and geometric confinement provided by the zeolite.
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