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Al-containing MCM-41 type materials were prepared by three different synthesis methods (aluminum grafting on the calcined MCM-41, pH adjustment during the crystallization period and crystallization in the presence of zeolite seeds). The samples were characterized by powder XRD, nitrogen adsorption, 27Al MAS NMR and FTIR with pyridine as probe molecule. All the samples exhibit a high hydrothermal stability at high temperature just with a minor structural degradation. N2 adsorption data obtained for the sample prepared from a gel containing zeolite seeds suggest a higher structural resistance to the hydrothermal treatment in comparison with the samples prepared by other methods. A different type of pyridine adsorbed, probably interacting simultaneously with a Brönsted and a Lewis acid site, is observed upon pyridine adsorption. This type...
Three different methods were used to introduce 1.0 wt.% of Pt in bifunctional Pt/MCM-22 zeolite catalysts: ion exchange with Pt(NH3)(4)(2+), incipient wetness impregnation with PtCl6H2 and mechanical mixture with Pt/Al2O3. The Pt dispersion was estimated by transmission electron microscopy and the hydrogenating activity with toluene hydrogenation at 110 degrees C. From these experiments, it can be concluded that with the ion exchanged sample, platinum was located within the inner micropores and on the outer surface, whereas with the impregnated one, platinum was essentially on the outer surface under the form of large particles. With all the samples there is a fast initial decrease in the activity for n-hexane hydroisomerisation at 250 degrees C. With exchanged and impregnated samples, this decrease is followed by a plateau, the activi...
The experimental conditions leading to the synthesis of pure and highly crystalline AlPO,-40, CoAPO-40, and ZnAPO-40 have been optimized. Although the preparation of these phases is favored by the presence of TMA+ in the synthesis gel, these ions have not been found incorporated in the final AFR structures. All materials have been characterized by powder XRD, t.g./d.s.c., SEM, EDX, 13C, 27AI, and 3’P solid-state n.m.r., diffuse reflectance u.v.-vis spectroscopy, FTi.r., and catalytic tests using the n-t-xylene isomerization as a model reaction. This multitechnique approach provides strong evidence for the framework incorporation of cobalt and zinc. The acid sites generated by the framework insertion of cobalt and zinc are stronger than those generated by the incorporation of silicon.
SAPO-40 exhibits five main OH species, describable as high-frequency ones (HF, at 3737, 3730, and 3724 cm-1) and low-frequency ones (LF1 and LF2, at 3559 and 3528 cm-1, respectively), the former probably sitting in 12-member-ring channels and the latter either in side pockets or eight-member-ring channels of the AFR structure. The low-temperature interaction of such OH species with CO shows that HF species have strictly similar acidity (comparable to that of HY zeolites), in contrast with previous results concerning H-transfer to NH3. The ease of interaction and the spectral features are in accord with the location in large cavities. The vibration of H-bonded hydroxyl has a noticeable structure with subbands. The interaction of CO with LF1 and LF2 species occurs with difficulty and yields nonlinear complexes because of the steric hindr...
Two-dimensional triple- and quintuple-quantum 27AI magic-angle spinning (MO MAS) n.m.r. spectra of microporous AIPO-40 and SAPOBO have been recorded at 9.4 and 14.1 T. The resolution of the 5Q spectra of AIPO-40 is amazing, at least 11 resonances being resolved. The 3lQ spectra further reveal the presence of 2 other much fainter peaks. Because the AIPO-40 aluminium sites have different quadrupole coupling constants the 9.4 T spectra are slightly better resolved than the 14.1 T spectra, suggesting that in MO n.m.r. it may sometimes be advantageous to work at lower magnetic fields. The 3Q spectra of SAPO-40 are poorly resolved displaying a main broad peak and two faint resonances. This is because the introduction of even a small amount of Si into the framework of AIPO-40 generates a distribution of Al sites and a dispersion of chemical s...
SAPO-40 exhibits strong acid sites, which catalyse the reaction of disproportionation of ethylbenzene. The distribution of diethylbenzene isomers suggests a high void volume in the structure of this molecular sieve.
The thermal and hydrothermal stability of SAPO-40 has been evaluated using the isomerization of m-xylene as model reaction. The characterization of the porosity was also studied and compared to other well known structures, namely Y zeolite, mordenite and ZSM-5. The structural changes that occur under thermal treatments influence the activity and selectivity of SAPO-40, while hydrothermal treatments do not significantly change those properties. The results confirm the high stability of SAPO-40 under thermal and hydrothermal treatments. Catalytic tests and adsorption of cyclohexane indicate that regular large side pockets or lobes exist along the main channels of SAPO-40, which create a large void volume responsible for the high rate of adsorption, high amount of adsorbed cyclohexane and the low shape selectivity in m-xylene isomerization.
Highly crystalline CoAPSO-40 and ZnAPSO-40 have been synthesized and characterized by powder XRD, TG/ DSC, SEM, EDX, 27Al, 31P and 29Si solid-state NMR, di use re¯ectance UV±VIS spectroscopy, FT IR and catalytic tests using the m-xylene isomerization and n-heptane cracking as model reactions. The simultaneous incorporation of silicon and a divalent metal in the framework of the AFR structure results in the generation of Brùnsted acid sites similar to those found in SAPO-40 and MeAPO-40. The catalytic activity of the samples for acid catalyzed reactions is higher than that of SAPO-40 with a homogeneous framework silicon distribution. The framework incorporation of cobalt or zinc results in a decrease of the thermal and hydrothermal stability of the metal bearing AFR framework, when compared with AlPO4-40 and SAPO-40.
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