Two bentonites from Paraíba (Northeastern Brazil) were impregnated with heteropoly phosphomolybdic H3PMo12O40 (HPMo). The materials produced were characterized by various techniques such as N2 adsorption-desorption (specific surface area, SSA), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Thermogravimetric analysis (TGA/DTG), Scanning Electron Microscopy (SEM) equipped with Dispersive Energy X-ray spectroscopy (EDS), ultraviolet-visible spectroscopy (UV-vis), acid-base titration analysis. The catalytic activity of these materials was tested in the esterification of a waste from palm oil deodorization and the main results obtained (about 93.3% of conversion) indicated that these materials have potential to act as heterogeneous solid acid catalysts. The prepared materials exhibited satisfactory catalytic performance even after a very simple recycling process in three reuse cycles, without significant loss of their activities.
The
synthesis of aluminosilicate Al-MCM-41 was performed using
mining kaolin waste as an alternative source of silicon and aluminum
to add value to this waste. In a preliminary stage, acid leaching
was carried out with the kaolin residue with three different durations
(1, 1.5 and 2 h) to evaluate the leaching time that provided the highest
amounts of silicon and aluminum in the tailings. Molecular sieves
were synthesized by the hydrothermal method and calcined at 550 °C
to eliminate the surfactant. X-ray diffractograms of the synthesized
samples revealed that the sample AM41-2H, obtained from kaolin leached
for 2 h (MC7-2H), presented the best structural arrangement due to
the presence of 2θ angles close to 2.32°, a specific surface
area of 1016 m2·g–1, a pore volume
of 0.80 cm3·g–1, and a pore diameter
of 3.14 nm, which are characteristic of Al-MCM-41. A sample of AM41-2H
was functionalized with 3-mercaptopropyltrimethoxysilane (MTPS) (5
mmol MTPS/g AM41-2H). To eliminate excess unaltered MTPS on the surface
of the material, the functionalized aluminosilicate (AM41-2H-F) was
subjected to a purification step. The organic functional group that
remained in the molecular sieve (−SH) was then oxidized to
its corresponding acid group (−SO3H) to form stronger
acid sites. Then, the heterogeneous catalyst obtained (AM41-2H-O)
was tested in an esterification reaction of oleic acid with methanol
and in an esterification reaction of an industrial waste from palm
oil refinement (DDPO), which is generated during the deodorization
process of palm oil. Both reactions were carried out for 2 h at 130
°C, with a fatty acid/methanol molar ratio of 1:30 and addition
of 5% catalyst to the mass of fatty acid. The results obtained revealed
that the conversion to esters from oleic acid and DDPO was 99% and
98%, respectively, in contrast to the uncatalyzed reaction, which
achieved only 15% conversion. The catalysts used in the reactions
were recovered and reused in the same conditions as the initial reactions,
which showed conversions in this first cycle of catalyst reuse of
98% for oleic acid and 81% for DDPO, proving the efficiency of the
catalyst synthesized from industrial kaolin waste.
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