Preparation and characterization of metallacalixarenes anchored to a mesoporous silica SBA-15 LP as potential catalysts

Jeff Espinas; Jeremie Pelletier; Kai C. Szeto; Nicolas Merle; Erwan Le Roux; Christine Lucas; Aimery De Mallmann; Jean Marie Basset; Mostafa Taoufik; Jean Thivolle-Cazat

doi:10.1016/j.micromeso.2013.12.031

Preparation and characterization of metallacalixarenes anchored to a mesoporous silica SBA-15 LP as potential catalysts

Jeff Espinas, Jeremie Pelletier, Kai C. Szeto, Nicolas Merle, Erwan Le Roux, Christine Lucas, Aimery De Mallmann, Jean Marie Basset, Mostafa Taoufik, Jean Thivolle-Cazat^*

^*Corresponding author for this work

Research output: Contribution to journal › Article › peer-review

10 Scopus citations

Abstract

The calixarene [[4H]-(OH)₃(H)] was used as a linker between a mesoporous silica SBA-15 LP (large pore) modified with Al(iBu) ₃·(Et₂O) and organometallic complexes Zr( ^{â̂ -}CH₂Ph)₄ or W(CtBu(CH ₂tBu)₃) to avoid steric and electronic interactions of the metallic centers with the oxide surface, and insure a better controlled coordination sphere. Hence, materials M1, [(SiO)₂AliBu· (Et₂O), Si-iBu]_{SBA-15 LP-(700)} and M2, [(SiO) ₂Al-[O-[4H]-(OH)₂(H)], Si-iBu]_{SBA-15 LP-(700)} were successively prepared by reaction of Al(i-Bu)₃·(Et ₂O) with the OH groups of SBA-15 LP treated at 700 C under vacuum, then with the calixarene [[4H]-(OH)₃(H)] at 25 C with a yield of 70%. M2 could then react with Zr(^{â̂ -}CH₂Ph) ₄ at 25 C and W(CtBu(CH₂tBu)₃) at 65 C to form the corresponding bipodal surface complexes on materials M3, [(SiO) ₂Al-[O-[4H]-(H)(O)₂Zr(^{â̂ -}CH ₂Ph)₂], Si-iBu]_{SBA-15 LP-(700)} and M4, [(SiO)₂Al-[O-[4H]-(H)(O)₂W(CtBu(CH₂tBu))], Si-iBu]_{SBA-15 LP-(700)} respectively. M4 proved to catalyze the propene metathesis with a high initial activity.

Original language	English (US)
Pages (from-to)	77-85
Number of pages	9
Journal	Microporous and Mesoporous Materials
Volume	188
DOIs	https://doi.org/10.1016/j.micromeso.2013.12.031
State	Published - Apr 2014

Keywords

Calixarene
Catalyst
Silica
Tungsten
Zirconium

ASJC Scopus subject areas

General Chemistry
General Materials Science
Condensed Matter Physics
Mechanics of Materials

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10.1016/j.micromeso.2013.12.031

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@article{949b1af3a19645a0a525dc990aeaef18,

title = "Preparation and characterization of metallacalixarenes anchored to a mesoporous silica SBA-15 LP as potential catalysts",

abstract = "The calixarene [[4H]-(OH)3(H)] was used as a linker between a mesoporous silica SBA-15 LP (large pore) modified with Al(iBu) 3·(Et2O) and organometallic complexes Zr( {\^a}̂ -CH2Ph)4 or W(CtBu(CH 2tBu)3) to avoid steric and electronic interactions of the metallic centers with the oxide surface, and insure a better controlled coordination sphere. Hence, materials M1, [(SiO)2AliBu· (Et2O), Si-iBu]SBA-15 LP-(700) and M2, [(SiO) 2Al-[O-[4H]-(OH)2(H)], Si-iBu]SBA-15 LP-(700) were successively prepared by reaction of Al(i-Bu)3·(Et 2O) with the OH groups of SBA-15 LP treated at 700 C under vacuum, then with the calixarene [[4H]-(OH)3(H)] at 25 C with a yield of 70%. M2 could then react with Zr({\^a}̂ -CH2Ph) 4 at 25 C and W(CtBu(CH2tBu)3) at 65 C to form the corresponding bipodal surface complexes on materials M3, [(SiO) 2Al-[O-[4H]-(H)(O)2Zr({\^a}̂ -CH 2Ph)2], Si-iBu]SBA-15 LP-(700) and M4, [(SiO)2Al-[O-[4H]-(H)(O)2W(CtBu(CH2tBu))], Si-iBu]SBA-15 LP-(700) respectively. M4 proved to catalyze the propene metathesis with a high initial activity.",

keywords = "Calixarene, Catalyst, Silica, Tungsten, Zirconium",

author = "Jeff Espinas and Jeremie Pelletier and Szeto, {Kai C.} and Nicolas Merle and {Le Roux}, Erwan and Christine Lucas and Mallmann, {Aimery De} and Basset, {Jean Marie} and Mostafa Taoufik and Jean Thivolle-Cazat",

year = "2014",

month = apr,

doi = "10.1016/j.micromeso.2013.12.031",

language = "English (US)",

volume = "188",

pages = "77--85",

journal = "Microporous and Mesoporous Materials",

issn = "1387-1811",

publisher = "Elsevier",

}

TY - JOUR

T1 - Preparation and characterization of metallacalixarenes anchored to a mesoporous silica SBA-15 LP as potential catalysts

AU - Espinas, Jeff

AU - Pelletier, Jeremie

AU - Szeto, Kai C.

AU - Merle, Nicolas

AU - Le Roux, Erwan

AU - Lucas, Christine

AU - Mallmann, Aimery De

AU - Basset, Jean Marie

AU - Taoufik, Mostafa

AU - Thivolle-Cazat, Jean

PY - 2014/4

Y1 - 2014/4

N2 - The calixarene [[4H]-(OH)3(H)] was used as a linker between a mesoporous silica SBA-15 LP (large pore) modified with Al(iBu) 3·(Et2O) and organometallic complexes Zr( â̂ -CH2Ph)4 or W(CtBu(CH 2tBu)3) to avoid steric and electronic interactions of the metallic centers with the oxide surface, and insure a better controlled coordination sphere. Hence, materials M1, [(SiO)2AliBu· (Et2O), Si-iBu]SBA-15 LP-(700) and M2, [(SiO) 2Al-[O-[4H]-(OH)2(H)], Si-iBu]SBA-15 LP-(700) were successively prepared by reaction of Al(i-Bu)3·(Et 2O) with the OH groups of SBA-15 LP treated at 700 C under vacuum, then with the calixarene [[4H]-(OH)3(H)] at 25 C with a yield of 70%. M2 could then react with Zr(â̂ -CH2Ph) 4 at 25 C and W(CtBu(CH2tBu)3) at 65 C to form the corresponding bipodal surface complexes on materials M3, [(SiO) 2Al-[O-[4H]-(H)(O)2Zr(â̂ -CH 2Ph)2], Si-iBu]SBA-15 LP-(700) and M4, [(SiO)2Al-[O-[4H]-(H)(O)2W(CtBu(CH2tBu))], Si-iBu]SBA-15 LP-(700) respectively. M4 proved to catalyze the propene metathesis with a high initial activity.

AB - The calixarene [[4H]-(OH)3(H)] was used as a linker between a mesoporous silica SBA-15 LP (large pore) modified with Al(iBu) 3·(Et2O) and organometallic complexes Zr( â̂ -CH2Ph)4 or W(CtBu(CH 2tBu)3) to avoid steric and electronic interactions of the metallic centers with the oxide surface, and insure a better controlled coordination sphere. Hence, materials M1, [(SiO)2AliBu· (Et2O), Si-iBu]SBA-15 LP-(700) and M2, [(SiO) 2Al-[O-[4H]-(OH)2(H)], Si-iBu]SBA-15 LP-(700) were successively prepared by reaction of Al(i-Bu)3·(Et 2O) with the OH groups of SBA-15 LP treated at 700 C under vacuum, then with the calixarene [[4H]-(OH)3(H)] at 25 C with a yield of 70%. M2 could then react with Zr(â̂ -CH2Ph) 4 at 25 C and W(CtBu(CH2tBu)3) at 65 C to form the corresponding bipodal surface complexes on materials M3, [(SiO) 2Al-[O-[4H]-(H)(O)2Zr(â̂ -CH 2Ph)2], Si-iBu]SBA-15 LP-(700) and M4, [(SiO)2Al-[O-[4H]-(H)(O)2W(CtBu(CH2tBu))], Si-iBu]SBA-15 LP-(700) respectively. M4 proved to catalyze the propene metathesis with a high initial activity.

KW - Calixarene

KW - Catalyst

KW - Silica

KW - Tungsten

KW - Zirconium

UR - http://www.scopus.com/inward/record.url?scp=84893052045&partnerID=8YFLogxK

U2 - 10.1016/j.micromeso.2013.12.031

DO - 10.1016/j.micromeso.2013.12.031

M3 - Article

AN - SCOPUS:84893052045

SN - 1387-1811

VL - 188

SP - 77

EP - 85

JO - Microporous and Mesoporous Materials

JF - Microporous and Mesoporous Materials

ER -

Preparation and characterization of metallacalixarenes anchored to a mesoporous silica SBA-15 LP as potential catalysts

Abstract

Keywords

ASJC Scopus subject areas

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