Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane

Autores
Fasce, Diana Patricia; Dell'Erba, Ignacio Esteban; Williams, Roberto Juan Jose
Año de publicación
2005
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
The hydrolytic condensation of organotrialkoxysilanes containing (β-hydroxy) tertiary amine groups generates a significant fraction of intramolecular cycles and leads to the formation of closed structures. The aim of this study was to investigate if their co-condensation with a tetraalkoxy silane would take place by predominant intramolecular cyclization steps, eventually leading to functionalized silicas that can be dissolved in appropriate solvents. Co-condensation of tetraethoxysilane (TEOS) with the organotrialkoxysilane derived from the reaction of N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane with phenyl glycidyl ether, was performed in the presence of HCOOH using a thermal cycle attaining 150 °C. For TEOS molar fractions lower than 0.7, soluble functionalized-silicas containing up to about 25 wt% of inorganic silica chemically bonded to bulky organic groups, could be synthesized. The glass transition temperature of the organic part was close to 25 °C; it was inferred that the inorganic part was vitrified at the maximum temperature of the selected thermal cycle (150 °C). Most of the Si atoms supplied by the trialkoxysilane were present in fully condensed structures (T3), while those supplied by TEOS were present mostly as Q3 and Q 4 structures. These soluble functionalized-silicas may be used to introduce silica as a reinforcement of a polymer network. An example is shown, using an epoxy-diamine formulation. The equivalent of 10 wt% silica could be incorporated to the final network at the expense of a reduction of 26 °C in its glass transition temperature.
Fil: Fasce, Diana Patricia. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Dell'Erba, Ignacio Esteban. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Williams, Roberto Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Materia
Functionalized Silica
Organic-Inorganic Hybrid Polymers
Tetraethoxysilane
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-nd/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/82535
Acceder
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oai_identifier_str oai:ri.conicet.gov.ar:11336/82535
network_acronym_str CONICETDig
repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilaneFasce, Diana PatriciaDell'Erba, Ignacio EstebanWilliams, Roberto Juan JoseFunctionalized SilicaOrganic-Inorganic Hybrid PolymersTetraethoxysilanehttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1https://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1The hydrolytic condensation of organotrialkoxysilanes containing (β-hydroxy) tertiary amine groups generates a significant fraction of intramolecular cycles and leads to the formation of closed structures. The aim of this study was to investigate if their co-condensation with a tetraalkoxy silane would take place by predominant intramolecular cyclization steps, eventually leading to functionalized silicas that can be dissolved in appropriate solvents. Co-condensation of tetraethoxysilane (TEOS) with the organotrialkoxysilane derived from the reaction of N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane with phenyl glycidyl ether, was performed in the presence of HCOOH using a thermal cycle attaining 150 °C. For TEOS molar fractions lower than 0.7, soluble functionalized-silicas containing up to about 25 wt% of inorganic silica chemically bonded to bulky organic groups, could be synthesized. The glass transition temperature of the organic part was close to 25 °C; it was inferred that the inorganic part was vitrified at the maximum temperature of the selected thermal cycle (150 °C). Most of the Si atoms supplied by the trialkoxysilane were present in fully condensed structures (T3), while those supplied by TEOS were present mostly as Q3 and Q 4 structures. These soluble functionalized-silicas may be used to introduce silica as a reinforcement of a polymer network. An example is shown, using an epoxy-diamine formulation. The equivalent of 10 wt% silica could be incorporated to the final network at the expense of a reduction of 26 °C in its glass transition temperature.Fil: Fasce, Diana Patricia. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaFil: Dell'Erba, Ignacio Esteban. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaFil: Williams, Roberto Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaElsevier2005-07info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/82535Fasce, Diana Patricia; Dell'Erba, Ignacio Esteban; Williams, Roberto Juan Jose; Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane; Elsevier; Polymer; 46; 17; 7-2005; 6649-66560032-3861CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/url/https://www.sciencedirect.com/science/article/pii/S0032386105005549info:eu-repo/semantics/altIdentifier/doi/10.1016/j.polymer.2005.05.019info:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-nd/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-10-15T14:53:05Zoai:ri.conicet.gov.ar:11336/82535instacron:CONICETInstitucionalhttp://ri.conicet.gov.ar/Organismo científico-tecnológicoNo correspondehttp://ri.conicet.gov.ar/oai/requestdasensio@conicet.gov.ar; lcarlino@conicet.gov.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:34982025-10-15 14:53:05.915CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane
title Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane
spellingShingle Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane
Fasce, Diana Patricia
Functionalized Silica
Organic-Inorganic Hybrid Polymers
Tetraethoxysilane
title_short Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane
title_full Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane
title_fullStr Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane
title_full_unstemmed Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane
title_sort Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane
dc.creator.none.fl_str_mv Fasce, Diana Patricia
Dell'Erba, Ignacio Esteban
Williams, Roberto Juan Jose
author Fasce, Diana Patricia
author_facet Fasce, Diana Patricia
Dell'Erba, Ignacio Esteban
Williams, Roberto Juan Jose
author_role author
author2 Dell'Erba, Ignacio Esteban
Williams, Roberto Juan Jose
author2_role author
author
dc.subject.none.fl_str_mv Functionalized Silica
Organic-Inorganic Hybrid Polymers
Tetraethoxysilane
topic Functionalized Silica
Organic-Inorganic Hybrid Polymers
Tetraethoxysilane
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv The hydrolytic condensation of organotrialkoxysilanes containing (β-hydroxy) tertiary amine groups generates a significant fraction of intramolecular cycles and leads to the formation of closed structures. The aim of this study was to investigate if their co-condensation with a tetraalkoxy silane would take place by predominant intramolecular cyclization steps, eventually leading to functionalized silicas that can be dissolved in appropriate solvents. Co-condensation of tetraethoxysilane (TEOS) with the organotrialkoxysilane derived from the reaction of N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane with phenyl glycidyl ether, was performed in the presence of HCOOH using a thermal cycle attaining 150 °C. For TEOS molar fractions lower than 0.7, soluble functionalized-silicas containing up to about 25 wt% of inorganic silica chemically bonded to bulky organic groups, could be synthesized. The glass transition temperature of the organic part was close to 25 °C; it was inferred that the inorganic part was vitrified at the maximum temperature of the selected thermal cycle (150 °C). Most of the Si atoms supplied by the trialkoxysilane were present in fully condensed structures (T3), while those supplied by TEOS were present mostly as Q3 and Q 4 structures. These soluble functionalized-silicas may be used to introduce silica as a reinforcement of a polymer network. An example is shown, using an epoxy-diamine formulation. The equivalent of 10 wt% silica could be incorporated to the final network at the expense of a reduction of 26 °C in its glass transition temperature.
Fil: Fasce, Diana Patricia. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Dell'Erba, Ignacio Esteban. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Williams, Roberto Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
description The hydrolytic condensation of organotrialkoxysilanes containing (β-hydroxy) tertiary amine groups generates a significant fraction of intramolecular cycles and leads to the formation of closed structures. The aim of this study was to investigate if their co-condensation with a tetraalkoxy silane would take place by predominant intramolecular cyclization steps, eventually leading to functionalized silicas that can be dissolved in appropriate solvents. Co-condensation of tetraethoxysilane (TEOS) with the organotrialkoxysilane derived from the reaction of N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane with phenyl glycidyl ether, was performed in the presence of HCOOH using a thermal cycle attaining 150 °C. For TEOS molar fractions lower than 0.7, soluble functionalized-silicas containing up to about 25 wt% of inorganic silica chemically bonded to bulky organic groups, could be synthesized. The glass transition temperature of the organic part was close to 25 °C; it was inferred that the inorganic part was vitrified at the maximum temperature of the selected thermal cycle (150 °C). Most of the Si atoms supplied by the trialkoxysilane were present in fully condensed structures (T3), while those supplied by TEOS were present mostly as Q3 and Q 4 structures. These soluble functionalized-silicas may be used to introduce silica as a reinforcement of a polymer network. An example is shown, using an epoxy-diamine formulation. The equivalent of 10 wt% silica could be incorporated to the final network at the expense of a reduction of 26 °C in its glass transition temperature.
publishDate 2005
dc.date.none.fl_str_mv 2005-07
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
http://purl.org/coar/resource_type/c_6501
info:ar-repo/semantics/articulo
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/11336/82535
Fasce, Diana Patricia; Dell'Erba, Ignacio Esteban; Williams, Roberto Juan Jose; Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane; Elsevier; Polymer; 46; 17; 7-2005; 6649-6656
0032-3861
CONICET Digital
CONICET
url http://hdl.handle.net/11336/82535
identifier_str_mv Fasce, Diana Patricia; Dell'Erba, Ignacio Esteban; Williams, Roberto Juan Jose; Synthesis of a soluble functionalized-silica by the hydrolysis and condensation of organotrialkoxysilanes bearing (β-hydroxy) tertiary amine groups with tetraethoxysilane; Elsevier; Polymer; 46; 17; 7-2005; 6649-6656
0032-3861
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/url/https://www.sciencedirect.com/science/article/pii/S0032386105005549
info:eu-repo/semantics/altIdentifier/doi/10.1016/j.polymer.2005.05.019
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-nd/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-nd/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
application/pdf
application/pdf
dc.publisher.none.fl_str_mv Elsevier
publisher.none.fl_str_mv Elsevier
dc.source.none.fl_str_mv reponame:CONICET Digital (CONICET)
instname:Consejo Nacional de Investigaciones Científicas y Técnicas
reponame_str CONICET Digital (CONICET)
collection CONICET Digital (CONICET)
instname_str Consejo Nacional de Investigaciones Científicas y Técnicas
repository.name.fl_str_mv CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicas
repository.mail.fl_str_mv dasensio@conicet.gov.ar; lcarlino@conicet.gov.ar
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score 13.221938

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