The influence of gel properties on the kinetics of crystallization and particulate properties of MFI-type zeolities. I. The influence of time and temperature of gel ageing on the particulate properties of silicalite-1 microcrystals

Microporous Materials Pub Date : 1997-12-01 DOI:10.1016/S0927-6513(97)00075-8

Ankica Čižmek , Boris Subotica , Damir Kralj , Vesna Babić-Ivančić , Anton Tonejc

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引用次数: 28

Abstract

The influence of time and temperature of ageing of the amorphous gel precursor (2.5Na₂O-8TPABr-60SiO₂-800H₂O) on the particulate properties (particle size distribution, particle shape, number of particles) of silicalite-1 synthesized at 170°C were studied by different experimental methods such as X-ray diffractometry (XRD), differential thermogravimetric analysis (TGA), particle size analysis, FT infra-red spectroscopy and scanning-electron microscopy (SEM). In spite of negligible changes in the crystal morphology, ageing of the gel considerably affects the number and size of silicalite-1 crystals in the crystalline end products. The observed effects were discussed in terms of the formation of specific ordered subunits between silicate species and TPA⁺ ions (germ nuclei) and their role in the nucleation and crystal growth of silicalite-1 crystals.

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凝胶性质对mfi型沸石结晶动力学和颗粒性质的影响。1 .凝胶老化时间和温度对硅石-1微晶颗粒性能的影响

采用x射线衍射(XRD)、差示热重分析(TGA)、粒度分析、红外光谱(FT)和扫描电镜(SEM)等实验方法，研究了在170℃下合成的非晶态凝胶前体(2.5 na20 - 8tpbr - 60sio2 - 800h2o)时效时间和温度对硅石-1颗粒性能(粒度分布、颗粒形状、颗粒数量)的影响。尽管晶体形态的变化可以忽略不计，但凝胶的老化极大地影响了结晶最终产品中硅石-1晶体的数量和大小。从TPA+离子(胚核)与硅酸盐之间特定有序亚基的形成及其在硅酸-1晶体成核和晶体生长中的作用等方面讨论了所观察到的效应。

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Microporous Materials

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Author index Subject index Contents Investigation of organosilanes as structure-directing agents in zeolite synthesis The influence of gel properties on the kinetics of crystallization and particulate properties of MFI-type zeolities. I. The influence of time and temperature of gel ageing on the particulate properties of silicalite-1 microcrystals