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A General Autofluorescence Method to Characterize Polymerization Progress.

Pía A López1, Vy H B Pham1, Suzanne A Blum1

  • 1Department of Chemistry, University of California, Irvine, Irvine, CA 92697-2025, USA.

Angewandte Chemie (International Ed. in English)
|May 19, 2023
PubMed
Summary
This summary is machine-generated.

This study introduces a novel autofluorescence technique to monitor polymerization in real-time, even for non-fluorescent materials like dicyclopentadiene. The method uses fluorescence lifetime recovery after photobleaching (FLRAP) to quantitatively track reaction progress.

Keywords:
AutofluorescenceFluorescence Lifetime Imaging Microscopy (FLIM)Fluorescence Lifetime Recovery after Photobleaching (FLRAP)Fluorescence SpectroscopyRing-Opening Polymerization

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Area of Science:

  • Polymer Chemistry
  • Materials Science
  • Spectroscopy

Background:

  • Traditional fluorescence spectroscopy requires specific fluorogenic groups on monomers or polymers, limiting its application.
  • Hydrocarbon-based monomers like dicyclopentadiene and their polymers lack inherent fluorescence handles.
  • Monitoring polymerization of such materials typically requires indirect methods.

Purpose of the Study:

  • To develop a real-time, in-line autofluorescence technique for monitoring polymerization progress.
  • To characterize polymerization of dicyclopentadiene/polydicyclopentadiene using native fluorescence properties.
  • To enable quantitative analysis of polymerization kinetics and formulation comparisons.

Main Methods:

  • Utilized ruthenium-catalyzed ring-opening metathesis polymerization (ROMP) of dicyclopentadiene.
  • Employed fluorescence recovery after photobleaching (FRAP) and a novel fluorescence lifetime recovery after photobleaching (FLRAP) method.
  • Correlated autofluorescence lifetime changes to the degree of cure and polymerization rates.

Main Results:

  • Autofluorescence lifetime recovery changes correlated linearly with the degree of cure during ROMP.
  • The method provided quantitative links to reaction progress without exogenous fluorophores.
  • Enabled relative rate comparisons for 10 different catalyst-inhibitor-stabilized formulations.
  • Demonstrated suitability for high-throughput evaluation of thermoset formulations.

Conclusions:

  • The combined autofluorescence and FLRAP/FRAP method offers a powerful tool for real-time polymerization monitoring of native systems.
  • This technique overcomes limitations of traditional fluorescence methods for non-fluorescent materials.
  • The approach is potentially extendable to other polymerization reactions lacking inherent fluorescence handles.