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The Effect of the ZrO2 Loading in SiO2@ZrO2-CaO Catalysts for Transesterification Reaction

机译:SiO2 @ ZrO2-CaO催化剂中ZrO2负载量对酯交换反应的影响

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摘要

The effect of the ZrO loading was studied on spherical SiO @ZrO -CaO structures synthetized by a simple route that combines the Stöber and sol-gel methods. The texture of these materials was determined using S by N adsorption, where the increment in SiO spheres’ surface areas was reached with the incorporation of ZrO . Combined the characterization techniques of using different alcoholic dissolutions of zirconium (VI) butoxide 0.04 M, 0.06 M, and 0.08 M, we obtained SiO @ZrO materials with 5.7, 20.2, and 25.2 wt % of Zr. Transmission electron microscopy (TEM) analysis also uncovered the shape and reproducibility of the SiO spheres. The presence of Zr and Ca in the core–shell was also determined by TEM. X-ray diffraction (XRD) profiles showed that the c-ZrO phase changed in to m-ZrO by incorporating calcium, which was confirmed by Raman spectroscopy. The purity of the SiO spheres, as well as the presence of Zr and Ca in the core–shell, was assessed by the Fourier transform infrared (FTIR) method. CO temperature programmed desorption (TPD-CO ) measurements confirmed the increment in the amount of the basic sites and strength of these basic sites due to calcium incorporation. The catalyst reuse in FAME production from canola oil transesterification allowed confirmation that these calcium core@shell catalysts turn out to be actives and stables for this reaction.
机译:研究了ZrO负载对通过结合了Stöber和溶胶-凝胶法的简单路线合成的球形SiO @ZrO -CaO结构的影响。这些材料的质构是通过S通过N吸附来确定的,其中掺入ZrO可以达到SiO球表面积的增加。结合使用0.04 M,0.06 M和0.08 M的丁醇锆(VI)的不同醇溶性的表征技术,我们获得了ZrO为5.7、20.2和25.2 wt%的SiO @ ZrO材料。透射电子显微镜(TEM)分析还揭示了SiO球的形状和可重复性。 TEM也确定了核壳中Zr和Ca的存在。 X射线衍射(XRD)图谱表明,通过掺入钙,c-ZrO相变成了m-ZrO,这通过拉曼光谱法得到证实。 SiO球的纯度以及核-壳中Zr和Ca的存在,通过傅里叶变换红外(FTIR)方法进行了评估。 CO温度程序解吸(TPD-CO)测量结果证实,由于钙的引入,碱性位点数量的增加和这些碱性位点的强度增加。在低芥酸菜子油酯交换反应的FAME生产中催化剂的重复使用可以确认这些钙核壳催化剂对于该反应而言是活性和稳定的。

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