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ENCAPSULATION OF Co PHTHALOCYANINE IN ALUMINA-PILLARED CLAYS AND THEIR CHARACTERIZATION

机译:酞菁钴在铝质黏土中的包封及其表征

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Alumina-pillared montmorillonite clays (Al-PILC), prepared under ultrasonic (US) agitation and normal stirring (S) methods, have been used as a host material to encapsulate Co phthalocyanine (CoPc) complex. The amount of Co varies from 0.27 to 1.48 wt.% in the samples, depending on the input concentration of Co. Powder X-ray diffraction and other characterization techniques reveal that the structure of Al-PILC remains intact after the incorporation of the complex into the pores through a pyridine solution of the complex by ultrasonic agitation. A substantial decrease in the BET surface area and total pore volume of Al-PILC points to the occupation of the CoPc moieties within the porous structure of the pillared clay. This is further supported by the observation of a band at 1489 cm~(-1) in the Fourier transform infrared (FTIR) spectra of the encapsulated samples. The FTIR and diffuse reflectance ultraviolet-visible (DRUV-Vis) spectral results indicate that the encapsulated CoPc complex in the clay matrix undergoes distortion in order to accommodate itself within the pores of the Al-PILC. The encapsulated samples prepared by ultrasonification show better dispersion of the complex than the samples prepared under normal stirring conditions. Compared to the 'neat' complex, the encapsulated samples (CoPc in Al-PILC) exhibit greater turnover in the test reaction of the oxidation of benzyl alcohol to benzaldehyde with tert-butyl hydroperoxide as the oxidant at 373 K. The method of preparation and consequent site isolation of CoPc in Al-PILC influence the catalytic activity.
机译:在超声(US)搅拌和常规搅拌(S)方法下制备的氧化铝柱状蒙脱土(Al-PILC)已用作包封钴酞菁(CoPc)配合物的主体材料。样品中Co的含量在0.27-1.48 wt。%之间变化,具体取决于Co的输入浓度。粉末X射线衍射和其他表征技术表明,将络合物掺入后,Al-PILC的结构保持完整通过超声搅拌使络合物的吡啶溶液通过孔。 Al-PILC的BET表面积和总孔体积的大幅减少表明,CoPc部分被带柱粘土的多孔结构所占据。在包封样品的傅立叶变换红外(FTIR)光谱中观察到1489 cm〜(-1)的谱带进一步证明了这一点。 FTIR和漫反射紫外可见(DRUV-Vis)光谱结果表明,粘土基质中封装的CoPc配合物会发生变形,以使其自身容纳在Al-PILC的孔中。与常规搅拌条件下制备的样品相比,通过超声法制备的包封样品显示出更好的配合物分散性。与“纯”配合物相比,被封装的样品(Al-PILC中的CoPc)在以叔丁基氢过氧化物为氧化剂在373 K的苄醇氧化为苯甲醛的测试反应中表现出更高的转化率。制备方法和因此,Al-PILC中CoPc的位点分离会影响催化活性。

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