Comparative studies of Zr-based MCM-41 and MCM-48 mesoporous molecular sieves: Synthesis and physicochemical properties
Two surfactant-templated synthetic routes are developed for the preparation of new types of mesoporous molecular sieves, Zr-MCM-41 and Zr-MCM-48, using different Si sources but keeping the same zirconium precursor (zirconium- n-propoxide). When fumed silica was used as Si precursor, a Zr-MCM-48 mate...
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Published in | Applied surface science Vol. 253; no. 5; pp. 2443 - 2451 |
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Main Authors | , , , , , , , , |
Format | Journal Article |
Language | English |
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Elsevier B.V
30.12.2006
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Abstract | Two surfactant-templated synthetic routes are developed for the preparation of new types of mesoporous molecular sieves, Zr-MCM-41 and Zr-MCM-48, using different Si sources but keeping the same zirconium precursor (zirconium-
n-propoxide). When fumed silica was used as Si precursor, a Zr-MCM-48 material of cubic structure was formed with a surface area of 654.8
m
2/g and an unimodal pore diameter distribution. It shows low stability: after calcination at 600
°C, the ordered structure was transformed into a relatively disordered worm-like mesostructure with many defects and silanol groups. The use of tetraethyl orthosilicate as Si source led to the formation of a Zr-MCM-41 mesoporous solid, which had good thermal stability and a highly ordered hexagonal arrangement, with a surface area 677.9
m
2/g and an uniform pore diameter distribution. Fourier transform infrared (FT-IR) characterization and
29Si NMR analysis confirm that zirconium ions indeed incorporated into the framework of the solid. The in situ FT-IR spectroscopy of pyridine adsorption reveals that both, Lewis and Brönsted acid sites, were formed on the surface of these mesoporous materials. The strength and number of the Brönsted acid sites of the Zr-MCM-48 solid were greater than those of the Zr-MCM-41, due to a lower degree of condensation reaction during the synthesis that led to more structural defects in the framework and more silanol groups stretching from the solid surface. |
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AbstractList | Two surfactant-templated synthetic routes are developed for the preparation of new types of mesoporous molecular sieves, Zr-MCM-41 and Zr-MCM-48, using different Si sources but keeping the same zirconium precursor (zirconium-
n-propoxide). When fumed silica was used as Si precursor, a Zr-MCM-48 material of cubic structure was formed with a surface area of 654.8
m
2/g and an unimodal pore diameter distribution. It shows low stability: after calcination at 600
°C, the ordered structure was transformed into a relatively disordered worm-like mesostructure with many defects and silanol groups. The use of tetraethyl orthosilicate as Si source led to the formation of a Zr-MCM-41 mesoporous solid, which had good thermal stability and a highly ordered hexagonal arrangement, with a surface area 677.9
m
2/g and an uniform pore diameter distribution. Fourier transform infrared (FT-IR) characterization and
29Si NMR analysis confirm that zirconium ions indeed incorporated into the framework of the solid. The in situ FT-IR spectroscopy of pyridine adsorption reveals that both, Lewis and Brönsted acid sites, were formed on the surface of these mesoporous materials. The strength and number of the Brönsted acid sites of the Zr-MCM-48 solid were greater than those of the Zr-MCM-41, due to a lower degree of condensation reaction during the synthesis that led to more structural defects in the framework and more silanol groups stretching from the solid surface. Two surfactant-templated synthetic routes are developed for the preparation of new types of mesoporous molecular sieves, Zr-MCM-41 and Zr-MCM-48, using different Si sources but keeping the same zirconium precursor (zirconium-n-propoxide). When fumed silica was used as Si precursor, a Zr-MCM-48 material of cubic structure was formed with a surface area of 654.8 m2/g and an unimodal pore diameter distribution. It shows low stability: after calcination at 600 DGC, the ordered structure was transformed into a relatively disordered worm-like mesostructure with many defects and silanol groups. The use of tetraethyl orthosilicate as Si source led to the formation of a Zr-MCM-41 mesoporous solid, which had good thermal stability and a highly ordered hexagonal arrangement, with a surface area 677.9 m2/g and an uniform pore diameter distribution. Fourier transform infrared (FT-IR) characterization and 29Si NMR analysis confirm that zirconium ions indeed incorporated into the framework of the solid. The in situ FT-IR spectroscopy of pyridine adsorption reveals that both, Lewis and Bronsted acid sites, were formed on the surface of these mesoporous materials. The strength and number of the Bronsted acid sites of the Zr-MCM-48 solid were greater than those of the Zr-MCM-41, due to a lower degree of condensation reaction during the synthesis that led to more structural defects in the framework and more silanol groups stretching from the solid surface. |
Author | Salas, P. Llanos, M.E. Noreña, L.E. Navarrete, J. Chen, L.F. Wang, J.A. Zhou, X.L. Montoya, A. Del Angel, P. |
Author_xml | – sequence: 1 givenname: L.F. surname: Chen fullname: Chen, L.F. email: chenlf2001@yahoo.com organization: Departamento de Ciencias Básicas, Universidad Autónoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 México D.F., Mexico – sequence: 2 givenname: X.L. surname: Zhou fullname: Zhou, X.L. organization: Petroleum Processing Research Center, East China University of Science and Technology, 200237 Shanghai, China – sequence: 3 givenname: L.E. surname: Noreña fullname: Noreña, L.E. email: lnf@correo.azc.uam.mx organization: Departamento de Ciencias Básicas, Universidad Autónoma Metropolitana-A, Av. San Pablo 180, Col. Reynosa-Tamaulipas, 02200 México D.F., Mexico – sequence: 4 givenname: J.A. surname: Wang fullname: Wang, J.A. organization: Laboratorio de Catálisis y Materiales, SEPI-ESIQIE, Instituto Politécnico Nacional, Av. Politécnico S/N, Col. Zacatenco, 07738 México D.F., Mexico – sequence: 5 givenname: J. surname: Navarrete fullname: Navarrete, J. organization: Grupo de Molecular Ingeniería, Instituto Mexicano del Petróleo, Eje Lázaro Cárdenas 152, 07730 México D.F., Mexico – sequence: 6 givenname: P. surname: Salas fullname: Salas, P. organization: Grupo de Molecular Ingeniería, Instituto Mexicano del Petróleo, Eje Lázaro Cárdenas 152, 07730 México D.F., Mexico – sequence: 7 givenname: A. surname: Montoya fullname: Montoya, A. organization: Grupo de Molecular Ingeniería, Instituto Mexicano del Petróleo, Eje Lázaro Cárdenas 152, 07730 México D.F., Mexico – sequence: 8 givenname: P. surname: Del Angel fullname: Del Angel, P. organization: Grupo de Molecular Ingeniería, Instituto Mexicano del Petróleo, Eje Lázaro Cárdenas 152, 07730 México D.F., Mexico – sequence: 9 givenname: M.E. surname: Llanos fullname: Llanos, M.E. organization: Grupo de Molecular Ingeniería, Instituto Mexicano del Petróleo, Eje Lázaro Cárdenas 152, 07730 México D.F., Mexico |
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Snippet | Two surfactant-templated synthetic routes are developed for the preparation of new types of mesoporous molecular sieves, Zr-MCM-41 and Zr-MCM-48, using... |
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SubjectTerms | Mesoporous solid Surface acidity Templated synthesis Zr-MCM-41 Zr-MCM-48 |
Title | Comparative studies of Zr-based MCM-41 and MCM-48 mesoporous molecular sieves: Synthesis and physicochemical properties |
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