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Effect of ultrasound on the structural and textural properties of copper-impregnated cerium-modified zirconium-pillared bentonite

机译:超声波对浸铜铈改性锆柱膨润土结构和组织性能的影响

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In this study, the synthesis of zirconium-pillared bentonite modified with cerium was performed via two different methods by the application of conventional and ultrasonic treatments during the intercalation stage. To synthesise copper-impregnated pillared clays by wet impregnation, cerium-modified zirconium-pillared clays were used as supportive materials after being calcined at 300℃. Ultrasonic treatment significantly decreased the required processing time compared with the conventional treatment of the synthesised pillared bentonites. Chemical analysis confirmed the incorporation of Zr~(4+), Ce~(4+) and Cu~(2+) species into the pillared bentonites. X-ray diffraction (XRD) patterns of zirconium- and cerium/zirconium-pillared bentonites prepared by conventional treatment show that one large d-spacing above 3.5 nm corresponds to the mesoporous delaminated part, and another small d-spacing above 1.7 nm is indicative of the microporous pillared part. Zirconium- and cerium/zirconium-pillared bentonites prepared via ultrasonic treatment exhibited similar results, with the same high d-spacing but with a second low-intensity d-spacing above 1.9 nm. The delaminated structures of the pillared bentonites synthesised by both methods were conserved after copper impregnation. Nitrogen-adsorption isotherm analysis showed that the textural characteristics of products synthesised by ultrasonic treatment were comparable to those of products synthesised by conventional treatment. Fourier-transform infrared spectroscopy (FTIR) analyses showed the presence of Brensted- and Lewis-acid sites, and zirconium-pillared clays synthesised by conventional treatment exhibited increased numbers of Bransted- and Lewis-acid sites after cerium addition and copper impregnation. However, the products synthesised by ultrasonic treatment exhibited an increased number of Bronsted- and Lewis-acid sites after cerium addition, but a decreased number of acid sites after copper impregnation.
机译:在这项研究中,在插层阶段通过常规和超声处理,通过两种不同的方法合成了铈修饰的锆柱状膨润土。为了通过湿法浸渍法合成铜浸渍柱状粘土,将铈改性的锆柱状粘土在300℃下煅烧后用作支撑材料。与合成的带柱膨润土的常规处理相比,超声波处理显着减少了所需的处理时间。化学分析证实了Zr〜(4 +),Ce〜(4+)和Cu〜(2+)物种掺入到柱状膨润土中。通过常规处理制备的锆和铈/锆/柱状膨润土的X射线衍射(XRD)图谱表明,大于3.5 nm的一个大d间距对应于介孔分层部分,而另一个大于1.7 nm的小d间距是指示性的的微孔柱状部分。通过超声处理制备的锆和铈/锆-柱状膨润土表现出相似的结果,具有相同的高d间距,但第二个低强度d间距高于1.9 nm。两种方法合成的柱状膨润土的分层结构在铜浸渍后均得以保留。氮吸附等温线分析表明,超声处理合成的产品的织构特性与常规处理合成的产品相当。傅里叶变换红外光谱(FTIR)分析表明存在Brensted-和Lewis-酸位点,并且通过常规处理合成的锆柱状粘土在添加铈和铜浸渍后显示出Bransted-和Lewis酸位点数量增加。然而,通过超声处理合成的产物在添加铈之后表现出增加的布朗斯台德和路易斯酸位点数量,但是在铜浸渍之后表现出减少的酸位点数量。

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