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首页> 外文期刊>Dalton transactions: An international journal of inorganic chemistry >A novel approach to characterization of a relatively unstable intercalation compound under ambient conditions: revisiting a kaolinite-acetone intercalation compound
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A novel approach to characterization of a relatively unstable intercalation compound under ambient conditions: revisiting a kaolinite-acetone intercalation compound

机译：在环境条件下表征相对不稳定的嵌入化合物的新方法：重新发现高岭石 - 丙酮嵌入化合物

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摘要

Characteristics of a kaolinite-acetone intercalation compound prepared using a kaolinite N-methylformamide intercalation compound (Kaol-NMF) as an intermediate were obtained by a set of techniques with attention to suppressing evaporation and deintercalation of acetone. X-ray diffraction (XRD) with spectroscopic analyses, Fourier-transform infrared spectroscopy (FTIR) accompanied by solid-state C-13 and Si-29 nuclear magnetic resonance (NMR) spectroscopy with cross polarization (CP) and magic angle spinning (MAS) enable us to demonstrate full replacement of a pre-intercalated NMF monolayer with an acetone monolayer between the layers of kaolinite with an increase in the basal spacing from 1.08 nm (Kaol-NMF) to 1.12 nm. In addition, the appearance of an additional OH stretching band at 3630 cm(-1) and the shift of the C O stretching band to a lower wavenumber, from 1714 to 1701 cm(-1), in the FTIR spectrum, along with a downfield shift of the signal due to C O groups from 209 ppm, where a singlet was observed in the liquid-state C-13 NMR spectrum of acetone in CDCl3, to 219 ppm in the C-13 CP/MAS NMR spectrum, indicate hydrogen bond formation between interlayer hydroxyl groups of kaolinite and C O groups of the intercalated acetone molecules. These careful characterization studies provide information on an interaction between kaolinite and acetone under ambient conditions.
机译：以高岭石N-甲基甲酰胺插层化合物（Kaol NMF）为中间体制备的高岭石-丙酮插层化合物的特性是通过一系列技术获得的，这些技术关注的是抑制丙酮的蒸发和脱层。X射线衍射（XRD）和光谱分析，傅里叶变换红外光谱（FTIR）以及交叉极化（CP）和魔角旋转（MAS）的固态C-13和Si-29核磁共振（NMR）光谱使我们能够证明高岭石层之间的预插层NMF单层完全被丙酮单层取代，基底间距从1.08 nm（Kaol NMF）增加到1.12纳米。此外，在FTIR光谱中，在3630厘米（-1）处出现了一个额外的OH拉伸带，并将CO拉伸带移动到较低的波数，从1714到1701厘米（-1），同时，由于CO基团，信号的下场移动从209 ppm（在CDCl3中丙酮的液态C-13 NMR光谱中观察到了单线态），到C-13 CP/MAS NMR光谱中的219 ppm，表明高岭石的层间羟基和插层丙酮分子的CO基团之间形成氢键。这些细致的表征研究提供了环境条件下高岭石和丙酮之间相互作用的信息。

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