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Synthesis and Characterization of Functionalized Silica Mesoporous Crystals: Cationic Surfactant and Co-structure Directing Agent System
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). (Prof. Osamu Terasaki's group)
2010 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This dissertation has been focused on the synthesis and characterization of novel functionalized silica mesoporous crystals by using cationic surfactant and co–structure directing agents (CSDA), the central concept of the synthesis method is to build proper organic/inorganic interactions by introducing CSDA into the synthesis system.

By using cationic surfactant as template and anionic CSDA, carboxylic group functionalized mesoporous silicas were successfully synthesized. Well ordered 2D p6mm, cubic Fm-3m, mixture of CCP (Fm-3m) and HCP (P63/mmc), and cubic Fd-3m with uniform carboxylic group distribution have been obtained. Besides, we have investigated the Fm-3m/Fd-3m type intergrowth and new type defects observed in the Fd-3m structure using transmission electron microscopy (TEM) and proposed a “polyhedron packing” model.

New amphoteric, inorganic amino acid with highly ordered mesopores were synthesized. Uniform distribution of acid and base organic groups on the mesopore surfaces were formed by interactions between the counter charged surfactant head groups and ionic parts of CSDAs. It has been demonstrated that organic (–NH2 and –COOH) pairs incorporated in the mesopore walls behave as natural amino acids, collectively exhibiting an isoelectric point of ~6.0. Moreover, we have demonstrated that the inorganic amino acid is an efficient catalyst for the reaction between aldehydes and carbon nucleophiles.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University , 2010. , 82 p.
Keyword [en]
Mesoporous silica, Template synthesis, Functionalization, Electron microscopy, Defects, Crystal growth, Catalysis
National Category
Inorganic Chemistry
Research subject
Structural Chemistry
Identifiers
URN: urn:nbn:se:su:diva-38398ISBN: 978-91-7447-029-1 (print)OAI: oai:DiVA.org:su-38398DiVA: diva2:310270
Public defence
2010-05-18, Magnélisalen, Kemiska övningslaboratoriet, Svante Arrhenius väg 16 B, Stockholm, 13:00 (English)
Opponent
Supervisors
Available from: 2010-04-26 Created: 2010-04-13 Last updated: 2010-04-14Bibliographically approved
List of papers
1. A lesson from the unusual morphology of silica mesoporous crystals: Growth and close packing of spherical micelles with multiple twinning
Open this publication in new window or tab >>A lesson from the unusual morphology of silica mesoporous crystals: Growth and close packing of spherical micelles with multiple twinning
2006 (English)In: Angewandte Chemie International Edition, ISSN 1433-7851, E-ISSN 1521-3773, Vol. 45, no 39, 6516-6519 p.Article in journal (Refereed) Published
Keyword
crystal growth, electron microscopy, mesoporous materials, silica, surfactants
Identifiers
urn:nbn:se:su:diva-25028 (URN)10.1002/anie.200601451 (DOI)
Note
Part of urn:nbn:se:su:diva-7651Available from: 2008-05-12 Created: 2008-05-09 Last updated: 2017-12-13Bibliographically approved
2. Synthesis of carboxylic group functionalized mesoporous silicas (CFMSs) with various structures
Open this publication in new window or tab >>Synthesis of carboxylic group functionalized mesoporous silicas (CFMSs) with various structures
Show others...
2007 (Swedish)In: Journal of Materials Chemistry, ISSN 0959-9428, E-ISSN 1364-5501, Vol. 17, 1216-1221 p.Article in journal (Refereed) Published
Identifiers
urn:nbn:se:su:diva-20822 (URN)10.1039/b615209k (DOI)000244869100010 ()
Available from: 2007-12-01 Created: 2007-12-01 Last updated: 2017-12-13Bibliographically approved
3. Synthesis and Characterization of the Amphoteric Amino Acid Bifunctional Mesoporous Silica
Open this publication in new window or tab >>Synthesis and Characterization of the Amphoteric Amino Acid Bifunctional Mesoporous Silica
Show others...
2007 (English)In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 19, no 11, 2860-2867 p.Article in journal (Refereed) Published
Identifiers
urn:nbn:se:su:diva-19813 (URN)10.1021/cm0705845 (DOI)000246645100025 ()
Available from: 2007-11-28 Created: 2007-11-28 Last updated: 2017-12-13Bibliographically approved
4. Structural Analyses of Intergrowth and Stacking Fault in Cage-Type Mesoporous Crystals
Open this publication in new window or tab >>Structural Analyses of Intergrowth and Stacking Fault in Cage-Type Mesoporous Crystals
2009 (English)In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 21, no 2, 223-229 p.Article in journal (Refereed) Published
Identifiers
urn:nbn:se:su:diva-36789 (URN)10.1021/cm802162r (DOI)000262605200008 ()
Available from: 2010-01-26 Created: 2010-01-26 Last updated: 2017-12-12Bibliographically approved
5. Insight Into the Defects of Cage-Type Silica Mesoporous Crystals with Fd(3)over-arm Symmetry: TEM Observations and a New Proposal of "Polyhedron Packing" for the Crystals  
Open this publication in new window or tab >>Insight Into the Defects of Cage-Type Silica Mesoporous Crystals with Fd(3)over-arm Symmetry: TEM Observations and a New Proposal of "Polyhedron Packing" for the Crystals  
2009 (English)In: Chemistry - A European Journal, ISSN 0947-6539, E-ISSN 1521-3765, Vol. 15, no 12, 2818-2825 p.Article in journal (Refereed) Published
Keyword
crystal growth, defects, electron microscopy, mesoporous materials, template synthesis
Identifiers
urn:nbn:se:su:diva-36782 (URN)10.1002/chem.200801688 (DOI)000264511500014 ()
Available from: 2010-01-26 Created: 2010-01-26 Last updated: 2017-12-12Bibliographically approved
6. An amphoteric mesoporous silica catalyzed aldol reaction
Open this publication in new window or tab >>An amphoteric mesoporous silica catalyzed aldol reaction
2009 (English)In: Catalysis communications, ISSN 1566-7367, E-ISSN 1873-3905, Vol. 10, no 10, 1386-1389 p.Article in journal (Refereed) Published
Abstract [en]

A bi-functional mesoporous silica material, containing both carboxylic acid and amino groups, acts as a catalyst for the reaction between aldehydes and carbon nucleophiles. We demonstrate reaction conditions under which even aldehydes containing deactivating electron donating groups, or sterically demanding substituents, undergo the catalyzed reaction with acetone, affording primarily the condensation products. Moreover, we demonstrate that acetophenone and ethyl methyl ketone can replace acetone as nucleophile. The bi-functional mesoporous silica is a convenient catalyst, as it is simple to remove from the reaction media, thereby facilitating workup.

Keyword
Mesoporous silica, Catalysis, Aldol reaction, Bi-functional materials
Identifiers
urn:nbn:se:su:diva-36707 (URN)10.1016/j.catcom.2009.03.001 (DOI)000265811500006 ()
Available from: 2010-01-25 Created: 2010-01-25 Last updated: 2017-12-12Bibliographically approved

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