Synthesis of branched poly(methyl methacrylate)s: Effect of the branching comonomer structure

F. Isaure, P.A.G. Cormack, D.C. Sherrington

Research output: Contribution to journalArticle

128 Citations (Scopus)

Abstract

Branched poly(methyl methacrylate)s have been prepared using conventional solution phase free radical polymerization of methyl methacrylate (MATA) in the presence of a branching divinyl comonomer with appropriate levels of dodecanethiol (DDT) chain transfer agent added to inhibit gelation. The branching comonomers employed were five ethylene glycol dimethacrylates with varying lengths of PEG chains, divinylbenzene (DVB), and ethylene glycol diacrylate (EGDA). Soluble branched polymers were obtained in good yield with a MMA/brancher mole ratio up to 100/15. The minimum mole ratio of DDT required to avoid gelation was evaluated. The isolated polymers were characterized by elemental analysis to determine the level of DDT incorporated, by H-1 NMR spectroscopy, to determine the molecular composition and in particular the level of brancher incorporated (both as a branch unit and as a pendant functionality), and by double detection SEC in order to evaluate the level of branching. The differing behaviors of the branchers are discussed with a focus on a comparison of ethylene glycol dimethacrylate (EGDMA), EGDA and DVB. The latter brancher has been shown to produce the most regularly branched material with the smallest molar mass distributions. In general, however, the latter are broad or very broad.
LanguageEnglish
Pages2096-2105
Number of pages9
JournalMacromolecules
Volume37
Issue number6
DOIs
Publication statusPublished - 23 Mar 2004

Fingerprint

divinyl benzene
Ethylene Glycol
Polymethyl Methacrylate
Gelation
Ethylene glycol
Polymethyl methacrylates
Polymers
Methacrylates
Molar mass
Free radical polymerization
Chemical analysis
Nuclear magnetic resonance spectroscopy
Polyethylene glycols
ethylene dimethacrylate

Keywords

  • CONDENSING VINYL POLYMERIZATION
  • FREE-RADICAL COPOLYMERIZATION
  • CHAIN TRANSFER AGENT
  • HYPERBRANCHED POLYMERS
  • METHYL-METHACRYLATE
  • FACILE SYNTHESIS
  • REACTIVITY
  • STAR

Cite this

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title = "Synthesis of branched poly(methyl methacrylate)s: Effect of the branching comonomer structure",
abstract = "Branched poly(methyl methacrylate)s have been prepared using conventional solution phase free radical polymerization of methyl methacrylate (MATA) in the presence of a branching divinyl comonomer with appropriate levels of dodecanethiol (DDT) chain transfer agent added to inhibit gelation. The branching comonomers employed were five ethylene glycol dimethacrylates with varying lengths of PEG chains, divinylbenzene (DVB), and ethylene glycol diacrylate (EGDA). Soluble branched polymers were obtained in good yield with a MMA/brancher mole ratio up to 100/15. The minimum mole ratio of DDT required to avoid gelation was evaluated. The isolated polymers were characterized by elemental analysis to determine the level of DDT incorporated, by H-1 NMR spectroscopy, to determine the molecular composition and in particular the level of brancher incorporated (both as a branch unit and as a pendant functionality), and by double detection SEC in order to evaluate the level of branching. The differing behaviors of the branchers are discussed with a focus on a comparison of ethylene glycol dimethacrylate (EGDMA), EGDA and DVB. The latter brancher has been shown to produce the most regularly branched material with the smallest molar mass distributions. In general, however, the latter are broad or very broad.",
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Synthesis of branched poly(methyl methacrylate)s: Effect of the branching comonomer structure. / Isaure, F.; Cormack, P.A.G.; Sherrington, D.C.

In: Macromolecules, Vol. 37, No. 6, 23.03.2004, p. 2096-2105.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Synthesis of branched poly(methyl methacrylate)s: Effect of the branching comonomer structure

AU - Isaure, F.

AU - Cormack, P.A.G.

AU - Sherrington, D.C.

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Y1 - 2004/3/23

N2 - Branched poly(methyl methacrylate)s have been prepared using conventional solution phase free radical polymerization of methyl methacrylate (MATA) in the presence of a branching divinyl comonomer with appropriate levels of dodecanethiol (DDT) chain transfer agent added to inhibit gelation. The branching comonomers employed were five ethylene glycol dimethacrylates with varying lengths of PEG chains, divinylbenzene (DVB), and ethylene glycol diacrylate (EGDA). Soluble branched polymers were obtained in good yield with a MMA/brancher mole ratio up to 100/15. The minimum mole ratio of DDT required to avoid gelation was evaluated. The isolated polymers were characterized by elemental analysis to determine the level of DDT incorporated, by H-1 NMR spectroscopy, to determine the molecular composition and in particular the level of brancher incorporated (both as a branch unit and as a pendant functionality), and by double detection SEC in order to evaluate the level of branching. The differing behaviors of the branchers are discussed with a focus on a comparison of ethylene glycol dimethacrylate (EGDMA), EGDA and DVB. The latter brancher has been shown to produce the most regularly branched material with the smallest molar mass distributions. In general, however, the latter are broad or very broad.

AB - Branched poly(methyl methacrylate)s have been prepared using conventional solution phase free radical polymerization of methyl methacrylate (MATA) in the presence of a branching divinyl comonomer with appropriate levels of dodecanethiol (DDT) chain transfer agent added to inhibit gelation. The branching comonomers employed were five ethylene glycol dimethacrylates with varying lengths of PEG chains, divinylbenzene (DVB), and ethylene glycol diacrylate (EGDA). Soluble branched polymers were obtained in good yield with a MMA/brancher mole ratio up to 100/15. The minimum mole ratio of DDT required to avoid gelation was evaluated. The isolated polymers were characterized by elemental analysis to determine the level of DDT incorporated, by H-1 NMR spectroscopy, to determine the molecular composition and in particular the level of brancher incorporated (both as a branch unit and as a pendant functionality), and by double detection SEC in order to evaluate the level of branching. The differing behaviors of the branchers are discussed with a focus on a comparison of ethylene glycol dimethacrylate (EGDMA), EGDA and DVB. The latter brancher has been shown to produce the most regularly branched material with the smallest molar mass distributions. In general, however, the latter are broad or very broad.

KW - CONDENSING VINYL POLYMERIZATION

KW - FREE-RADICAL COPOLYMERIZATION

KW - CHAIN TRANSFER AGENT

KW - HYPERBRANCHED POLYMERS

KW - METHYL-METHACRYLATE

KW - FACILE SYNTHESIS

KW - REACTIVITY

KW - STAR

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T2 - Macromolecules

JF - Macromolecules

SN - 0024-9297

IS - 6

ER -