Copper species were incorporated into SBA-15 by solid-state grinding precursor with as-prepared mesoporous silica (SPA). The obtained materials (CuAS) were well-characterized by XRD, TEM, N(2) adsorption, H(2)-TPR, IR, and TG and compared with the material derived from calcined SBA-15 (CuCS). Surprisingly, CuO up to 6.7 mmol·g(-1) can be highly dispersed on SBA-15 by use of SPA strategy. Such CuO forms a smooth layer coated on the internal walls of SBA-15, which contributes to the spatial order and results in less-blocked mesopores. However, the aggregation of CuO takes place in CuCS material containing 6.7 mmol·g(-1) copper, which generates large CuO particles of 21.4 nm outside the mesopores. We reveal that the high dispersion extent of CuO is ascribed to the abundant silanols, as well as the confined space between template and silica walls provided by as-prepared SBA-15. The SPA strategy allows template removal and precursor conversion in one step, avoids the repeated calcination in conventional modification process, and saves time and energy. We also demonstrate that the CuAS material after autoreduction exhibits much better adsorptive desulfurization capacity than CuCS. Moreover, the adsorption capacity of regenerated adsorbent can be recovered completely.
By use of a surfactant templating method, the direct synthesis of magnesia-incorporated mesoporous alumina (mMgAl-γ) was realized via self-assembly of inexpensive inorganic salts. The structural and basic properties of the obtained materials were well characterized by various approaches. The results show that mMgAl-γ samples possess strong basicity with excellent water-resistant ability, well-defined mesoporous structure, and γ-Al2O3 crystalline frameworks. In comparison with wet impregnation that leads to structural damage, the direct synthesis strategy allows the mesoporous alumina to maintain good mesostructure. For example, the Brunauer−Emmett−Teller surface area of sample mMgAl(0.1)-γ can reach 328 m2·g−1, which is obviously higher than that of the sample prepared by a conventional impregnation method (239 m2·g−1). Further investigations evidence that the fabrication of suitable preassembled mesoporous precursors is crucial for the efficiency of the present direct synthesis strategy. In the process of calcination, the strongly basic species MgO was produced simultaneously and in situ coated on newly formed mesoporous γ-Al2O3 from preassembled precursors. Besides mMgAl-γ, mesoporous γ-Al2O3 materials functionalized with iron, chromium, and lead oxides were also successfully prepared, which demonstrates the generality of the strategy.
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