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Synthesis and homopolymerization kinetics of 7-(methacroyloxy)-2-oxo-heptylphosphonic acid and its copolymerization with methyl methacrylate.

ABSTRACT: The synthesis of polymerizable 7-(methacroyloxy)-2-oxo-heptylphosphonic acid M1 destined for self-etch adhesives is described. M1 is characterized by 1H, 13C and 31P-NMR spectroscopy. Its homopolymerization and copolymerization reactivity in the solvents methanol and dioxane between 45 and 70°C in the presence of azobisisobutyronitrile (AIBN) are examined. Polymerization proceeds readily through a thermal free radical initiation. The intensity exponents for the monomer and initiator are only slightly over 1 and approximately 0.5, respectively. This is in accordance with the results typically observed for an ideal free radical polymerization with termination mainly by disproportionation, which is typical for methyl methacrylate (MMA) homopolymerization. The kinetics of copolymerization with MMA are monitored by online 1H-NMR spectroscopy. Two copolymerization reactions for each pair of co-monomers are sufficient to evaluate the copolymerization parameters using the Jaacks method, the Fineman-Ross method and the nonlinear least-squares method. All three methods give similar results for particular monomer M1/MMA couple.

SUBMITTER: Chmela S

PROVIDER: S-EPMC6419686 | biostudies-literature | 2019

REPOSITORIES: biostudies-literature

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Synthesis and homopolymerization kinetics of 7-(methacroyloxy)-2-oxo-heptylphosphonic acid and its copolymerization with methyl methacrylate.

Chmela Štefan Š Fiedlerová Agnesa A Liptaj Tibor T Catel Yohann Y Moszner Norbert N

Designed monomers and polymers 20190308 1

The synthesis of polymerizable 7-(methacroyloxy)-2-oxo-heptylphosphonic acid M1 destined for self-etch adhesives is described. M1 is characterized by 1H, 13C and 31P-NMR spectroscopy. Its homopolymerization and copolymerization reactivity in the solvents methanol and dioxane between 45 and 70°C in the presence of azobisisobutyronitrile (AIBN) are examined. Polymerization proceeds readily through a thermal free radical initiation. The intensity exponents for the m ...[more]

PMID: 30890902

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Project description:A series of poly(lauryl methacrylate)-poly(methyl methacrylate-stat-lauryl methacrylate) (PLMA x -P(MMA-stat-LMA) y ) diblock copolymer nanoparticles were synthesized via RAFT dispersion copolymerization of 90 mol % methyl methacrylate (MMA) with 10 mol % lauryl methacrylate (LMA) in mineral oil by using a poly(lauryl methacrylate) (PLMA) precursor with a mean degree of polymerization (DP) of either 22 or 41. In situ 1H NMR studies of the copolymerization kinetics suggested an overall comonomer conversion of 94% within 2.5 h. GPC analysis confirmed a relatively narrow molecular weight distribution (M w/M n ≤ 1.35) for each diblock copolymer. Recently, we reported an unexpected morphology constraint when targeting PLMA22-PMMA y nano-objects in mineral oil, with the formation of kinetically trapped spheres being attributed to the relatively high glass transition temperature (T g) of the PMMA block. Herein we demonstrate that this limitation can be overcome by (i) incorporating 10 mol % LMA into the core-forming block and (ii) performing such syntheses at 115 °C. This new strategy produced well-defined spheres, worms, or vesicles when using the same PLMA22 precursor. Introducing the LMA comonomer not only enhances the mobility of the core-forming copolymer chains by increasing their solvent plasticization but also reduces their effective glass transition temperature to well below the reaction temperature. Copolymer morphologies were initially assigned via transmission electron microscopy (TEM) studies and subsequently confirmed via small-angle X-ray scattering analysis. The thermoresponsive behavior of PLMA22-P(0.9MMA-stat-0.1LMA)113 worms and PLMA22-P(0.9MMA-stat-0.1LMA)228 vesicles was also studied by using dynamic light scattering (DLS) and TEM. The former copolymer underwent a worm-to-sphere transition on heating from 20 to 170 °C while a vesicle-to-worm transition was observed for the latter. Such thermal transitions were irreversible at 0.1% w/w solids but proved to be reversible at 20% w/w solids.

Dataset Information

Synthesis and homopolymerization kinetics of 7-(methacroyloxy)-2-oxo-heptylphosphonic acid and its copolymerization with methyl methacrylate.

Publications

Synthesis and homopolymerization kinetics of 7-(methacroyloxy)-2-oxo-heptylphosphonic acid and its copolymerization with methyl methacrylate.

Similar Datasets

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