Journal article
Monitoring bulk acrylate-methacrylate photopolymerization reaction kinetics using in situ NMR
Polymer (Guilford), Vol.346, 129645
02/20/2026
DOI: 10.1016/j.polymer.2026.129645
Abstract
Herein, we use an in situ NMR technique to monitor both solvated and solvent-free photopolymerization reactions benefitting from the rich chemical information and high spectral resolution inherent to NMR. By placing an LED-coupled fiber optic and locking solvent within a concentric capillary situated inside the NMR tube, the photoreaction remains isolated from the solvent, allowing for the monitoring of bulk polymerizations. To optimize acquisition parameters, the relationship between nuclear relaxation and resin viscosity was investigated as a function of monomer conversion. The utility of this technique was explored by monitoring monomer conversion in photocurable hexyl acrylate, revealing remarkable reproducibility and agreement with kinetic theory. Additionally, double bond conversion in a photopolymer hydrogel was measured to illustrate the effect of monomer loading on reaction rate. Lastly, the high resolution of in situ NMR was employed to independently monitor the disappearance of acrylate and methacrylate double bonds in copolymerization reactions, directly demonstrating the preferential consumption of methacrylate over acrylate reactive groups.
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•In situ NMR was used to monitor solvent-free photopolymerization kinetics.•Concentric inner capillary isolated resin from locking solvent.•Acrylate/methacrylate conversion were independently tracked.•High reproducibility and agreement with kinetic theory.
Details
- Title: Subtitle
- Monitoring bulk acrylate-methacrylate photopolymerization reaction kinetics using in situ NMR
- Creators
- Luis L. Jessen - University of IowaNaomi Elmer - Brigham Young UniversityGeorge Crull - University of IowaKameron R. Hansen - University of IowaC. Allan Guymon - Brigham Young University
- Resource Type
- Journal article
- Publication Details
- Polymer (Guilford), Vol.346, 129645
- DOI
- 10.1016/j.polymer.2026.129645
- ISSN
- 0032-3861
- eISSN
- 1873-2291
- Publisher
- Elsevier Ltd
- Grant note
- Industry/University Cooperative Research Center (I/UCRC) for Fundamentals and Applications of Photopolymerization
Financial support for this work was provided by the Industry/University Cooperative Research Center (I/UCRC) for Fundamentals and Applications of Photopolymerization. We would like to express our sincere gratitude to the Polymer Chemistry and Technology group at TU Wien for performing the simultaneous IR/Rheology experiments that were essential to this work.
- Language
- English
- Date published
- 02/20/2026
- Academic Unit
- Chemistry; Chemical and Biochemical Engineering
- Record Identifier
- 9985134449902771
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