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THERMO-X-RAY-DIFFRACTION ANALYSIS OFDIMETHYLSULFOXIDE-KAOLINITE INTERCALATION COMPLEXES

机译:二甲基亚砜-高岭石插层复合物的热X射线衍射分析

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摘要

DMSO-kaolinite complexes of low- and high-defect Georgia kaolinite (KGa-1 and KGa-2, respectively) were investigated bythermo-XRD-analysis. X-ray patterns showed that DMSO was intercalated in both kaolinites with a d(001)-value of 1.11 nm (type Icomplex). The samples were gradually heated up to 170℃ and diffracted by X-ray at room-temperature. With the rise in temperature,due to the thermal evolution of the guest molecules, the relative intensity of the 1.11 nm peak decreased and that of the 0.72 nm peak(neat kaolinite) increased indicating that the fraction of the non-intercalated tactoids increased. The 1.11 peak disappeared at130-140℃. During the thermal treatment of both complexes two additional peaks appeared at 110 and 120℃, respectively, with d-val-ues of 0.79-0.94 and 0.61-0.67 nm in DMSO-KGa-1 and 0.81-0.86 and 0.62-0.66 nm in DMSO-KGa-2, indicating the formation of anew phase (type II complex). The new complex was obtained by the dehydration of type I complex and was composed of intercalatedDMSO molecules which did not escape. The new peaks disappeared at 150-160°C indicating the complete escape of DMSO.
机译:通过热XRD分析研究了低缺陷和高缺陷乔治亚高岭石(分别为KGa-1和KGa-2)的DMSO高岭石复合物。 X射线图显示DMSO插在两种高岭石中,其d(001)值为1.11 nm(Icomplex型)。将样品逐渐加热至170℃,并在室温下通过X射线衍射。随着温度的升高,由于客体分子的热演化,1.11 nm峰的相对强度降低,而0.72 nm峰(纯高岭石)的相对强度增加,这表明非插层触针的比例增加。 1.11峰在130-140℃消失。在两种配合物的热处理过程中,分别在110和120℃出现两个峰,在DMSO-KGa-1中的d值分别为0.79-0.94和0.61-0.67 nm,在DMSO-KGa-1中的d值分别为0.81-0.86和0.62-0.66 nm。 DMSO-KGa-2,表明形成了新相(II型复合物)。新的复合物是通过I型复合物的脱水作用而获得的,它由无法逸出的嵌入DMSO分子组成。新峰在150-160°C时消失,表明DMSO完全逸出。

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