High resolution solid-state NMR studies of polymer chemical and physical structures

Tonelli, Alan E.

doi:10.1007/978-94-011-2150-7_5

NMR Spectroscopy of Polymers 1993

DOI: 10.1007/978-94-011-2150-7_5

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High resolution solid-state NMR studies of polymer chemical and physical structures

Alan E. Tonelli¹

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Cited by 4 publications

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13C-NMR study on cure-accelerated phenol-formaldehyde resins with carbonates

Park

Riedl

2000

J. Appl. Polym. Sci.

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Both liquid-and solid-state 13 C-NMR spectroscopies were employed to investigate the cure-acceleration effects of three carbonates [propylene carbonate (PC), sodium carbonate (NC), and potassium carbonate (KC)] on liquid and cured phenolformaldehyde (PF) resins. The liquid-phase 13 C-NMR spectra showed that the cureacceleration mechanism in the PC-added PF resin seemed to be involved in increasing reactivity of the phenol rings, while the addition of both NC and KC into PF resin apparently resulted in the presence of ortho-ortho methylene linkages. Proton spinlattice rotating frame relaxation time (T 1H ) measured by solid-state 13 C-CP/MAS-NMR spectroscopy was smaller for the cure-accelerated PF resins than for that of the control PF resin. The result indicated that cure-accelerated PF resins are less rigid than the control PF resin.

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13C-NMR study on cure-accelerated phenol-formaldehyde resins with carbonates

Park

Riedl

2000

J. Appl. Polym. Sci.

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13C-NMR study on cure-accelerated phenol-formaldehyde resins with carbonates

Park

Riedl

2000

J. Appl. Polym. Sci.

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Both liquid‐ and solid‐state carbon‐13–nuclear magnetic resonance (13C‐NMR) spectroscopies were used to investigate the cure acceleration effects of three carbonates (propylene carbonate, sodium carbonate, and potassium carbonate) on liquid and cured phenol‐formaldehyde (PF) resins. The liquid‐phase 13C‐NMR spectra showed that the cure acceleration mechanism in the propylene carbonate‐added PF resin seemed to be involved in increasing reactivity of the phenol rings, whereas the addition of both sodium carbonate and potassium carbonate into PF resin apparently resulted in the presence of ortho–ortho methylene linkages. Proton spin‐lattice rotating frame relaxation time (T1ρH) measured by solid‐state 13C cross polarization/magic‐angle spinning NMR spectroscopy was smaller for the cure‐accelerated PF resins than that of the control PF resin. The result indicated that the cure‐accelerated PF resins are less rigid than the control PF resin. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 77: 1284–1293, 2000

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Enzymatic ring‐opening polymerization of ε‐caprolactone by a new lipase from Yarrowia lipolytica

Barrera-Rivera

Flores-Carreón

Martínez‐Richa

2008

J of Applied Polymer Sci

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A new lipase from the yeast Yarrowia lipolytica was isolated and used in the enzymatic ring-opening polymerization of lactones. The effect of used commercial oil from a vacuum pump (instead of olive oil) and in the presence of wheat flour was evaluated. It was found that lipase production is favored when wheat flour and used commercial oil is added instead of olive oil with an incubation time of 16.5 h at 298C and 250 rpm. Lipase shows a specific activity of 3.47 nmoles of 4-methyl umbelliferone released/mg of protein/min. In this way, preculture step can be avoided and an important reduction in production time can be obtained. In vitro polymerization of e-caprolactone at different temperatures in the presence of n-heptane for 15 days produces low-molecular-weight polyesters with unique multiphase morphology. Polyesters were characterized by NMR (solution and solid-state) spectroscopy, differential scanning calorimetry (DSC), Fourier-transformed infrared, wide-angle X-ray scattering and MALDI-TOF. Polyester crystallinities calculated by DSC were high, as expected for low-molecular-weight PCLs. Final polymer possesses carboxylic acid and hydroxyl end-groups, as determined by 1 H-and 13 C NMR analysis.

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High resolution solid-state NMR studies of polymer chemical and physical structures

Cited by 4 publications

References 42 publications

13C-NMR study on cure-accelerated phenol-formaldehyde resins with carbonates

13C-NMR study on cure-accelerated phenol-formaldehyde resins with carbonates

13C-NMR study on cure-accelerated phenol-formaldehyde resins with carbonates

Enzymatic ring‐opening polymerization of ε‐caprolactone by a new lipase from Yarrowia lipolytica

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