Monitoring the progress of a branching polymethylmethacrylate reaction via online rapid gel permeation chromatography (GPC) analysis

Peter Cormack, G. Saunders, D. Sherrington, P. Cormack, S. Graham, S. O'Donohue and J. McConville

Research output: Chapter in Book/Report/Conference proceedingConference contribution book

Abstract

A new methodology has been developed for the one-pot synthesis of a branched polymethyl methacrylate material. Employing a cross-linking comonomer and large amount of a chain transfer agent, a fully soluble material is produced through a conventional free radical reaction. It is thought that despite the presence of the cross-linker, a network is not formed due to the high chain transfer agent concentration instead resulting in a soluble polymer with a highly branched structure. Branched polymers are of interest for their unusual flow and viscometric properties, and this material is particularly attractive due to the relatively cheap and simple synthetic route. To better understand the mechanism of the reaction, an online monitoring system, the PL-PMC, was used to monitor the contents of the reactor at near real time during the polymerisation. A continuous stream of sample from the reactor was diluted to an appropriated level and injected into a rapid GPC analysis system comprising a differential refractive index detector, an online viscometer and a short GPC column to allow measurements in a ‘flow injection analysis’ mode. Measurements of bulk molecular weight and intrinsic viscosity parameters were made during synthesis, allowing the growth of the polymer to be closely followed. From the intrinsic viscosity measurements, the development of the branched structure was investigated as a function of reaction time. The final product was then isolated and investigated by offline analytical multi detector GPC to complete the study. Combining the data from the online monitoring investigation and the offline analysis of the final product, considerable insights into the reaction process were obtained from a single reaction.
LanguageEnglish
Title of host publicationProceedings of the world polymer congress (MACRO2006), 41st international symposium on macromolecules
EditorsAilton de Souza Gomes
Publication statusPublished - 2006
Event41st International Symposium on Macromolecules - IUPAC World Polymer Congress MACRO 2006 - Rio de Janeiro, Brazil
Duration: 16 Jul 200621 Jul 2006

Conference

Conference41st International Symposium on Macromolecules - IUPAC World Polymer Congress MACRO 2006
CountryBrazil
CityRio de Janeiro
Period16/07/0621/07/06

Fingerprint

Gel permeation chromatography
Polymethyl Methacrylate
Polymers
Monitoring
Free radical reactions
Detectors
Viscometers
Viscosity measurement
Refractive index
Molecular weight
Polymerization
Viscosity

Keywords

  • progress
  • polymethylmethacrylate reaction
  • analysis
  • rapid gel permeation chromatography
  • GPC

Cite this

G. Saunders, D. Sherrington, P. Cormack, S. Graham, S. O'Donohue and J. McConville (2006). Monitoring the progress of a branching polymethylmethacrylate reaction via online rapid gel permeation chromatography (GPC) analysis. In A. de Souza Gomes (Ed.), Proceedings of the world polymer congress (MACRO2006), 41st international symposium on macromolecules
G. Saunders, D. Sherrington, P. Cormack, S. Graham, S. O'Donohue and J. McConville. / Monitoring the progress of a branching polymethylmethacrylate reaction via online rapid gel permeation chromatography (GPC) analysis. Proceedings of the world polymer congress (MACRO2006), 41st international symposium on macromolecules. editor / Ailton de Souza Gomes. 2006.
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abstract = "A new methodology has been developed for the one-pot synthesis of a branched polymethyl methacrylate material. Employing a cross-linking comonomer and large amount of a chain transfer agent, a fully soluble material is produced through a conventional free radical reaction. It is thought that despite the presence of the cross-linker, a network is not formed due to the high chain transfer agent concentration instead resulting in a soluble polymer with a highly branched structure. Branched polymers are of interest for their unusual flow and viscometric properties, and this material is particularly attractive due to the relatively cheap and simple synthetic route. To better understand the mechanism of the reaction, an online monitoring system, the PL-PMC, was used to monitor the contents of the reactor at near real time during the polymerisation. A continuous stream of sample from the reactor was diluted to an appropriated level and injected into a rapid GPC analysis system comprising a differential refractive index detector, an online viscometer and a short GPC column to allow measurements in a ‘flow injection analysis’ mode. Measurements of bulk molecular weight and intrinsic viscosity parameters were made during synthesis, allowing the growth of the polymer to be closely followed. From the intrinsic viscosity measurements, the development of the branched structure was investigated as a function of reaction time. The final product was then isolated and investigated by offline analytical multi detector GPC to complete the study. Combining the data from the online monitoring investigation and the offline analysis of the final product, considerable insights into the reaction process were obtained from a single reaction.",
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G. Saunders, D. Sherrington, P. Cormack, S. Graham, S. O'Donohue and J. McConville 2006, Monitoring the progress of a branching polymethylmethacrylate reaction via online rapid gel permeation chromatography (GPC) analysis. in A de Souza Gomes (ed.), Proceedings of the world polymer congress (MACRO2006), 41st international symposium on macromolecules. 41st International Symposium on Macromolecules - IUPAC World Polymer Congress MACRO 2006, Rio de Janeiro, Brazil, 16/07/06.

Monitoring the progress of a branching polymethylmethacrylate reaction via online rapid gel permeation chromatography (GPC) analysis. / G. Saunders, D. Sherrington, P. Cormack, S. Graham, S. O'Donohue and J. McConville.

Proceedings of the world polymer congress (MACRO2006), 41st international symposium on macromolecules. ed. / Ailton de Souza Gomes. 2006.

Research output: Chapter in Book/Report/Conference proceedingConference contribution book

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AU - Cormack, Peter

AU - G. Saunders, D. Sherrington, P. Cormack, S. Graham, S. O'Donohue and J. McConville

PY - 2006

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N2 - A new methodology has been developed for the one-pot synthesis of a branched polymethyl methacrylate material. Employing a cross-linking comonomer and large amount of a chain transfer agent, a fully soluble material is produced through a conventional free radical reaction. It is thought that despite the presence of the cross-linker, a network is not formed due to the high chain transfer agent concentration instead resulting in a soluble polymer with a highly branched structure. Branched polymers are of interest for their unusual flow and viscometric properties, and this material is particularly attractive due to the relatively cheap and simple synthetic route. To better understand the mechanism of the reaction, an online monitoring system, the PL-PMC, was used to monitor the contents of the reactor at near real time during the polymerisation. A continuous stream of sample from the reactor was diluted to an appropriated level and injected into a rapid GPC analysis system comprising a differential refractive index detector, an online viscometer and a short GPC column to allow measurements in a ‘flow injection analysis’ mode. Measurements of bulk molecular weight and intrinsic viscosity parameters were made during synthesis, allowing the growth of the polymer to be closely followed. From the intrinsic viscosity measurements, the development of the branched structure was investigated as a function of reaction time. The final product was then isolated and investigated by offline analytical multi detector GPC to complete the study. Combining the data from the online monitoring investigation and the offline analysis of the final product, considerable insights into the reaction process were obtained from a single reaction.

AB - A new methodology has been developed for the one-pot synthesis of a branched polymethyl methacrylate material. Employing a cross-linking comonomer and large amount of a chain transfer agent, a fully soluble material is produced through a conventional free radical reaction. It is thought that despite the presence of the cross-linker, a network is not formed due to the high chain transfer agent concentration instead resulting in a soluble polymer with a highly branched structure. Branched polymers are of interest for their unusual flow and viscometric properties, and this material is particularly attractive due to the relatively cheap and simple synthetic route. To better understand the mechanism of the reaction, an online monitoring system, the PL-PMC, was used to monitor the contents of the reactor at near real time during the polymerisation. A continuous stream of sample from the reactor was diluted to an appropriated level and injected into a rapid GPC analysis system comprising a differential refractive index detector, an online viscometer and a short GPC column to allow measurements in a ‘flow injection analysis’ mode. Measurements of bulk molecular weight and intrinsic viscosity parameters were made during synthesis, allowing the growth of the polymer to be closely followed. From the intrinsic viscosity measurements, the development of the branched structure was investigated as a function of reaction time. The final product was then isolated and investigated by offline analytical multi detector GPC to complete the study. Combining the data from the online monitoring investigation and the offline analysis of the final product, considerable insights into the reaction process were obtained from a single reaction.

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KW - polymethylmethacrylate reaction

KW - analysis

KW - rapid gel permeation chromatography

KW - GPC

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M3 - Conference contribution book

BT - Proceedings of the world polymer congress (MACRO2006), 41st international symposium on macromolecules

A2 - de Souza Gomes, Ailton

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G. Saunders, D. Sherrington, P. Cormack, S. Graham, S. O'Donohue and J. McConville. Monitoring the progress of a branching polymethylmethacrylate reaction via online rapid gel permeation chromatography (GPC) analysis. In de Souza Gomes A, editor, Proceedings of the world polymer congress (MACRO2006), 41st international symposium on macromolecules. 2006