Influence of calcination temperature on the activity of mesoporous CaO/TiO 2–ZrO 2 catalyst in the esterification reaction

摘要

In the present study, the effect of calcination temperature on the structure and performance of mesoporous CaO/TiO~(2)–ZrO~(2)catalyst fabricated by sol–gel method used in the esterification reaction was assessed. Then, CaO/TiO~(2)catalyst was also synthesized via the same method to evaluate the effect of zirconia cations on its properties and activity. The samples were characterized by X-ray Diffraction?(XRD), Fourier transmittance infra-red (FT-IR), Brunauer–Emmett–Teller?(BET)–Barrett-Joyner-Halenda?(BJH), scanning electron microscope (SEM)?and transmission electron microscopy?(TEM) analyses. Moreover, Hammett indicator method was utilized to assess the acidity and basicity of the samples. It was found that zirconium was clearly incorporated in CaO/TiO~(2)lattice and transformed that from amorphous phase to crystalline structure. In addition, the basicity and acidity of CaO/TiO~(2)was clearly increased by zirconia loading. Evaluation of the samples’ activity presented that CaO/TiO~(2)catalyst exhibit no activity in the esterification reaction, while all CaO/TiO~(2)–ZrO~(2)catalysts showed high ability to convert oleic acid to its ester. Moreover, the catalyst calcined at 400?°C showed the highest activity in the esterification reaction with desirable properties such as high crystallinity, acidity, basicity and surface area along with well-distribution of particle size and pore size. The best catalyst converted around 90% of oleic acid to ester at optimized conditions of 150?°C, 12:1 molar ratio of methanol/oleic acid, 3?wt% of catalyst for 4?h of reaction time. Moreover, the sample was successfully used for five runs without significant reduction in activity that makes it a suitable choice as a catalyst for industrial applications. Graphical abstract.