Controlled epoxidation of poly(styrene-b-isoprene-b-styrene) block copolymer for the development of nanostructured epoxy thermosets
To be used as templates for nanostructured thermosets, a commercial poly(styrene-b-isoprene-b-styrene) (SIS) block copolymer (BCP) was epoxidized by three different epoxidation procedures. An exhaustive analysis of methodologies using metal catalyzed/hydrogen peroxide, dimethyldioxirane (DMDO), and...
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paper:paper_0887624X_v49_n20_p4505_Garate2023-06-08T15:46:54Z Controlled epoxidation of poly(styrene-b-isoprene-b-styrene) block copolymer for the development of nanostructured epoxy thermosets Goyanes, Silvia Nair D'Accorso, Norma Beatriz block copolymers dimethyldioxirane epoxidation nanocomposites phase separation thermosets Atomic force microscopy Catalysis Crosslinking Epoxidation Isoprene Nanocomposites Oxidation Peroxides Phase separation Styrene Thermosets Chromatographic techniques Diglycidyl ether of bisphenol-A Dimethyldioxirane Epoxy thermosets Macro phase separation Metal-catalyzed Nano-structured Nanostructured thermosets Block copolymers To be used as templates for nanostructured thermosets, a commercial poly(styrene-b-isoprene-b-styrene) (SIS) block copolymer (BCP) was epoxidized by three different epoxidation procedures. An exhaustive analysis of methodologies using metal catalyzed/hydrogen peroxide, dimethyldioxirane (DMDO), and meta-chloroperbenzoic acid (m-CPBA) was performed to obtain reactive BCPs. The DMDO approach was the best strategy to obtain highly epoxidized SIS BCP (85 mol %) without formation of side products. Careful control in BCP epoxidation by metal catalyzed/hydrogen peroxide and m-CPBA approaches led to a maximum epoxidation degree (ED) of approximately 60 mol % without the formation of side products. The ED by metal catalyzed/hydrogen peroxide strategy could be further increased to 69 mol %, but a significant amount of crosslinking, ring opening, and polymer chain scission reactions were detected by spectroscopic and chromatographic techniques. The miscibility of epoxidized BCPs with diglycidyl ether of bisphenol-A epoxy system before and after curing was analyzed to develop nanostructured epoxy thermosets. For ED higher than 69 mol %, BCPs were miscible, while those with lower ED presented macrophase separation. Highly epoxidized BCPs obtained by the DMDO methodology were successfully used to obtain ordered nanodomains inside the epoxy matrix, as determined by atomic force microscopy. © 2011 Wiley Periodicals, Inc. Fil:Goyanes, S. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales; Argentina. Fil:D'Accorso, N.B. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales; Argentina. 2011 https://bibliotecadigital.exactas.uba.ar/collection/paper/document/paper_0887624X_v49_n20_p4505_Garate http://hdl.handle.net/20.500.12110/paper_0887624X_v49_n20_p4505_Garate |
institution |
Universidad de Buenos Aires |
institution_str |
I-28 |
repository_str |
R-134 |
collection |
Biblioteca Digital - Facultad de Ciencias Exactas y Naturales (UBA) |
topic |
block copolymers dimethyldioxirane epoxidation nanocomposites phase separation thermosets Atomic force microscopy Catalysis Crosslinking Epoxidation Isoprene Nanocomposites Oxidation Peroxides Phase separation Styrene Thermosets Chromatographic techniques Diglycidyl ether of bisphenol-A Dimethyldioxirane Epoxy thermosets Macro phase separation Metal-catalyzed Nano-structured Nanostructured thermosets Block copolymers |
spellingShingle |
block copolymers dimethyldioxirane epoxidation nanocomposites phase separation thermosets Atomic force microscopy Catalysis Crosslinking Epoxidation Isoprene Nanocomposites Oxidation Peroxides Phase separation Styrene Thermosets Chromatographic techniques Diglycidyl ether of bisphenol-A Dimethyldioxirane Epoxy thermosets Macro phase separation Metal-catalyzed Nano-structured Nanostructured thermosets Block copolymers Goyanes, Silvia Nair D'Accorso, Norma Beatriz Controlled epoxidation of poly(styrene-b-isoprene-b-styrene) block copolymer for the development of nanostructured epoxy thermosets |
topic_facet |
block copolymers dimethyldioxirane epoxidation nanocomposites phase separation thermosets Atomic force microscopy Catalysis Crosslinking Epoxidation Isoprene Nanocomposites Oxidation Peroxides Phase separation Styrene Thermosets Chromatographic techniques Diglycidyl ether of bisphenol-A Dimethyldioxirane Epoxy thermosets Macro phase separation Metal-catalyzed Nano-structured Nanostructured thermosets Block copolymers |
description |
To be used as templates for nanostructured thermosets, a commercial poly(styrene-b-isoprene-b-styrene) (SIS) block copolymer (BCP) was epoxidized by three different epoxidation procedures. An exhaustive analysis of methodologies using metal catalyzed/hydrogen peroxide, dimethyldioxirane (DMDO), and meta-chloroperbenzoic acid (m-CPBA) was performed to obtain reactive BCPs. The DMDO approach was the best strategy to obtain highly epoxidized SIS BCP (85 mol %) without formation of side products. Careful control in BCP epoxidation by metal catalyzed/hydrogen peroxide and m-CPBA approaches led to a maximum epoxidation degree (ED) of approximately 60 mol % without the formation of side products. The ED by metal catalyzed/hydrogen peroxide strategy could be further increased to 69 mol %, but a significant amount of crosslinking, ring opening, and polymer chain scission reactions were detected by spectroscopic and chromatographic techniques. The miscibility of epoxidized BCPs with diglycidyl ether of bisphenol-A epoxy system before and after curing was analyzed to develop nanostructured epoxy thermosets. For ED higher than 69 mol %, BCPs were miscible, while those with lower ED presented macrophase separation. Highly epoxidized BCPs obtained by the DMDO methodology were successfully used to obtain ordered nanodomains inside the epoxy matrix, as determined by atomic force microscopy. © 2011 Wiley Periodicals, Inc. |
author |
Goyanes, Silvia Nair D'Accorso, Norma Beatriz |
author_facet |
Goyanes, Silvia Nair D'Accorso, Norma Beatriz |
author_sort |
Goyanes, Silvia Nair |
title |
Controlled epoxidation of poly(styrene-b-isoprene-b-styrene) block copolymer for the development of nanostructured epoxy thermosets |
title_short |
Controlled epoxidation of poly(styrene-b-isoprene-b-styrene) block copolymer for the development of nanostructured epoxy thermosets |
title_full |
Controlled epoxidation of poly(styrene-b-isoprene-b-styrene) block copolymer for the development of nanostructured epoxy thermosets |
title_fullStr |
Controlled epoxidation of poly(styrene-b-isoprene-b-styrene) block copolymer for the development of nanostructured epoxy thermosets |
title_full_unstemmed |
Controlled epoxidation of poly(styrene-b-isoprene-b-styrene) block copolymer for the development of nanostructured epoxy thermosets |
title_sort |
controlled epoxidation of poly(styrene-b-isoprene-b-styrene) block copolymer for the development of nanostructured epoxy thermosets |
publishDate |
2011 |
url |
https://bibliotecadigital.exactas.uba.ar/collection/paper/document/paper_0887624X_v49_n20_p4505_Garate http://hdl.handle.net/20.500.12110/paper_0887624X_v49_n20_p4505_Garate |
work_keys_str_mv |
AT goyanessilvianair controlledepoxidationofpolystyrenebisoprenebstyreneblockcopolymerforthedevelopmentofnanostructuredepoxythermosets AT daccorsonormabeatriz controlledepoxidationofpolystyrenebisoprenebstyreneblockcopolymerforthedevelopmentofnanostructuredepoxythermosets |
_version_ |
1768544555452334080 |