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Synthesis of high-quality MCM-48 mesoporous silica using gemini surfactant dimethylene-1,2-bis(dodecyldimethylammonium bromide)

机译:双子表面活性剂二亚甲基-1,2-双(十二烷基二甲基溴化铵)合成高质量mCm-48介孔二氧化硅

摘要

Using the Gemini surfactant [C12H25N+(CH3)(2-)N+(CH3)(2)-N+(CH3)(2)-C12H25](.)2Br(-) (abbreviated as C12-2-12) with the short spacer group (s = 2) as structure-directing agent and sodium silicate as precursor, high-quality ordered cubic mesoporous silica (space group Ia3d) was prepared through the S+I- route (S denotes surfactant, I precursor). The samples were characterized by small-angle X-ray diffraction, transmission electron microscopy, and N-2 adsorption-desorption techniques. Results showed that the pore structure of the resulting mesoporous silica belonged to the cubic structure (space group Ia3d). The high-quality cubic mesoporous structure was formed at 1:0.33 (molar ratio of sodium silicate to C12-2-12), 2:1 (ethyl acetate to sodium silicate), and at 30 degreesC. The formation conditions of MCM-48 with C12-2-12 were milder than those with the corresponding monovalent surfactants, such as alkyltrimethylammonium bromide. N-2 adsorption-desorption curves revealed type IV isotherms and H1 hysteresis loops; Brunauer-Emmet-Teller (BET) surface areas increased with the decrease of the molar ratio of sodium silicate to C12-2-12 and of ethyl acetate to sodium silicate as well as of the hydrothermal temperatures.
机译:使用Gemini表面活性剂[C12H25N +(CH3)(2-)N +(CH3)(2)-N +(CH3)(2)-C12H25](。)2Br(-)(缩写为C12-2-12)间隔基团(s = 2)作为结构导向剂,硅酸钠作为前体,通过S + I途径制备了高质量的有序立方介孔二氧化硅(空间群Ia3d)(S表示表面活性剂,I前体)。通过小角度X射线衍射,透射电子显微镜和N-2吸附-脱附技术对样品进行表征。结果表明,所得的中孔二氧化硅的孔结构属于立方结构(空间群Ia3d)。在1:0.33(硅酸钠与C12-2-12的摩尔比),2:1(乙酸乙酯与硅酸钠的摩尔比)和30℃下形成高质量的立方介孔结构。具有C12-2-12的MCM-48的形成条件比具有相应一价表面活性剂(如烷基三甲基溴化铵)的条件温和。 N-2吸附-解吸曲线显示IV型等温线和H1磁滞回线。 Brunauer-Emmet-Teller(BET)的表面积随硅酸钠与C12-2-12的摩尔比和乙酸乙酯与硅酸钠的摩尔比以及水热温度的降低而增加。

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