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Efficient assembly of hierarchical NaY aggregates by using an organosilane modified SDA
Microporous and Mesoporous Materials ( IF 5.2 ) Pub Date : 2018-01-10 , DOI: 10.1016/j.micromeso.2018.01.009
Xiaomeng Zhao , Xiaoling Meng , Yunshan Shang , Yu Song , Rugeng Liu , Jianhui Wei , Yanjun Gong , Zhihong Li

We demonstrate an efficient method for the assembly of hierarchical NaY aggregates by using a modified structure-directing agent (SDA) in an extremely dense aqueous system at 373K. By introducing the dimethylhexadecyl[3-(trimethoxysilyl)propyl] ammonium chloride (TPHAC) into the aluminosilicate sol, an organo-modified sol was formed and after ageing it was used as SDA in the feedstock gel to generate the well-aligned hierarchical NaY aggregates. The structure evolution of sol and formation of NaY aggregates were systematically investigated by FT-IR, XRD, SEM, TEM and synchrotron radiation small angel X-ray scattering (SR-SAXS), which confirmed the dominant impact of the organosilane on the aluminosilicate species and further on the outcome of the NaY aggregates. The results show that by adding the minimal amount of TPHAC in the sol, the sol promotes long period structure, forming a large amount of aluminosilicate species with suitable size and distribution, which are responsible for tuning the morphology and properties of NaY aggregates under the dense synthetic system. The typical NaY aggregate has high SiO2/Al2O3 of 5.3, consisting of particles (2–4 μm) orderly assembled from 20 to 80 nm crystalline domains of NaY zeolites with high pore volume of 0.43 cm3/g and external surface area of 100 m2/g. The morphology, crystal sizes, mesopore sizes, volume ratios of mesopore/micropore of NaY aggregate can be adjusted by varying the amount of TPHAC, the reaction time and solid content in the dense system. The new insight into regulating sol species structure by TPHAC and forming NaY crystal aggregates were discussed.



中文翻译:

通过使用有机硅烷改性的SDA高效组装NaY分层聚集体

我们展示了一种高效的方法,用于在373K的极其稠密的含水系统中使用修饰的结构导向剂(SDA)来组装NaY分层聚集体。通过将二甲基十六烷基[3-(三甲氧基甲硅烷基)丙基]氯化铵(TPHAC)引入铝硅酸盐溶胶中,形成有机改性溶胶,并在老化后将其用作原料凝胶中的SDA,以生成排列整齐的分层NaY聚集体。 。通过FT-IR,XRD,SEM,TEM和同步辐射小天使X射线散射(SR-SAXS)系统研究了溶胶的结构演变和NaY聚集体的形成,这证实了有机硅烷对硅铝酸盐物种的主要影响。以及关于NaY总量的结果。结果表明,通过在溶胶中添加最小量的TPHAC,溶胶促进了长周期结构,形成了大量具有合适尺寸和分布的硅铝酸盐物种,这些元素负责调节致密合成系统中NaY团聚体的形态和性能。典型的NaY骨料具有高SiO2 / Al 2 O 3为5.3,由20至80 nm的NaY沸石晶域有序组装的颗粒(2-4μm)组成,其高孔体积为0.43 cm 3 / g,外表面积为100 m 2 / g 。NaY聚集体的形态,晶体尺寸,中孔尺寸,中孔/微孔的体积比可以通过改变TPHAC的量,反应时间和致密体系中的固体含量来调节。讨论了通过TPHAC调节溶胶物种结构和形成NaY晶体聚集体的新见解。

更新日期:2018-01-10
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