Synthesis, thiol-yne "click" photopolymerization, and physical properties of networks derived from novel multifunctional alkynes

Multifunctional alkynes (2, 3, or 4 ynes per monomer) were prepared utilizing the nucleophile-catalyzed thio-Michael addition reaction from commercially available multifunctional thiols (2, 3, or 4 thiols) and propargyl acrylate. Real-time FTIR (RTIR) and NMR spectroscopies indicate that the conjuga...

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Main Authors: Chan, J., Shin, J., Hoyle, C., Bowman, C., Lowe, Andrew
Format: Journal Article
Published: American Chemical Society 2010
Online Access:http://hdl.handle.net/20.500.11937/46502
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author Chan, J.
Shin, J.
Hoyle, C.
Bowman, C.
Lowe, Andrew
author_facet Chan, J.
Shin, J.
Hoyle, C.
Bowman, C.
Lowe, Andrew
author_sort Chan, J.
building Curtin Institutional Repository
collection Online Access
description Multifunctional alkynes (2, 3, or 4 ynes per monomer) were prepared utilizing the nucleophile-catalyzed thio-Michael addition reaction from commercially available multifunctional thiols (2, 3, or 4 thiols) and propargyl acrylate. Real-time FTIR (RTIR) and NMR spectroscopies indicate that the conjugate addition under these conditions proceeds to high conversions within seconds using the nucleophilic catalyst dimethylphenylphosphine, in the absence of solvent, at ambient temperature, and with no side products. A family of polymer networks was prepared by the photoinitiated thiol-yne reaction employing a 2:1 ratio of thiol to alkyne, which resulted in uniformly cross-linked materials of systematically increasing cross-link density. Photopolymerization kinetic profiles indicate that the thiol-yne reaction proceeded rapidly to high conversion with conversions decreasing with increasing functionality of the thiol and/or alkyne groups. Differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) results clearly indicate that the glass transition temperature increases as the overall cross-link density increases (from -10 to 42 °C by DMTA). An increase in the rubbery modulus (from 6 to 23 MPa at 70 °C) results as the functionality increases, with a concomitant decrease in the molecular weight between cross-links. © 2010 American Chemical Society.
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spelling curtin-20.500.11937-465022017-09-13T13:39:37Z Synthesis, thiol-yne "click" photopolymerization, and physical properties of networks derived from novel multifunctional alkynes Chan, J. Shin, J. Hoyle, C. Bowman, C. Lowe, Andrew Multifunctional alkynes (2, 3, or 4 ynes per monomer) were prepared utilizing the nucleophile-catalyzed thio-Michael addition reaction from commercially available multifunctional thiols (2, 3, or 4 thiols) and propargyl acrylate. Real-time FTIR (RTIR) and NMR spectroscopies indicate that the conjugate addition under these conditions proceeds to high conversions within seconds using the nucleophilic catalyst dimethylphenylphosphine, in the absence of solvent, at ambient temperature, and with no side products. A family of polymer networks was prepared by the photoinitiated thiol-yne reaction employing a 2:1 ratio of thiol to alkyne, which resulted in uniformly cross-linked materials of systematically increasing cross-link density. Photopolymerization kinetic profiles indicate that the thiol-yne reaction proceeded rapidly to high conversion with conversions decreasing with increasing functionality of the thiol and/or alkyne groups. Differential scanning calorimetry (DSC) and dynamic mechanical thermal analysis (DMTA) results clearly indicate that the glass transition temperature increases as the overall cross-link density increases (from -10 to 42 °C by DMTA). An increase in the rubbery modulus (from 6 to 23 MPa at 70 °C) results as the functionality increases, with a concomitant decrease in the molecular weight between cross-links. © 2010 American Chemical Society. 2010 Journal Article http://hdl.handle.net/20.500.11937/46502 10.1021/ma1004452 American Chemical Society restricted
spellingShingle Chan, J.
Shin, J.
Hoyle, C.
Bowman, C.
Lowe, Andrew
Synthesis, thiol-yne "click" photopolymerization, and physical properties of networks derived from novel multifunctional alkynes
title Synthesis, thiol-yne "click" photopolymerization, and physical properties of networks derived from novel multifunctional alkynes
title_full Synthesis, thiol-yne "click" photopolymerization, and physical properties of networks derived from novel multifunctional alkynes
title_fullStr Synthesis, thiol-yne "click" photopolymerization, and physical properties of networks derived from novel multifunctional alkynes
title_full_unstemmed Synthesis, thiol-yne "click" photopolymerization, and physical properties of networks derived from novel multifunctional alkynes
title_short Synthesis, thiol-yne "click" photopolymerization, and physical properties of networks derived from novel multifunctional alkynes
title_sort synthesis, thiol-yne "click" photopolymerization, and physical properties of networks derived from novel multifunctional alkynes
url http://hdl.handle.net/20.500.11937/46502