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Exploiting Online Spatially Resolved Dynamic Light Scattering and Flow-NMR for Automated Size Targeting of
Peter M Pittaway1, Kudakwashe E Chingono1, Stephen T Knox1
1School of Chemical and Process Engineering, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, U.K.
ACS Polymers Au
|February 17, 2025
Summary
Automated flow reactors enable programmable synthesis of polymer nanoparticles with controlled sizes using reversible addition-fragmentation chain-transfer (RAFT) dispersion polymerization. Real-time monitoring ensures consistent production for diverse applications.
Area of Science:
- Polymer chemistry and materials science
- Nanotechnology and materials engineering
- Chemical engineering and process automation
Background:
- Polymer nanoparticles are crucial in various fields, but precise control over their size during synthesis remains challenging.
- Polymerization-induced self-assembly (PISA) offers a route to well-defined polymer architectures.
- Reversible addition-fragmentation chain-transfer (RAFT) dispersion polymerization is a key PISA technique.
Purpose of the Study:
- To develop an automated flow-reactor platform for programmable synthesis of polymer nanoparticles with controlled diameters.
- To integrate real-time monitoring techniques for process control and scale-up.
- To demonstrate the platform's utility in producing nanoparticles of specific sizes for discovery, development, and manufacture.
Main Methods:
- Utilized an automated flow-reactor system for polymerization-induced self-assembly (PISA) via RAFT dispersion polymerization.
- Employed inline spatially resolved dynamic light scattering (SRDLS) for real-time particle size measurement.
- Integrated benchtop nuclear magnetic resonance (NMR) spectroscopy for monitoring monomer conversion and kinetics.
Main Results:
- Achieved programmable synthesis of poly(N,N-dimethylacrylamide)-b-poly(diacetone acrylamide) (PDMAm-b-PDAAm) nanoparticles with specified diameters (50, 60, 70, 80 nm).
- Established a relationship between copolymer block length and nanoparticle size through initial training experiments.
- Demonstrated real-time process monitoring and control, ensuring product consistency during continuous manufacture.
Conclusions:
- The automated flow-reactor platform enables precise control over polymer nanoparticle synthesis.
- Inline SRDLS and NMR provide critical data for real-time monitoring and process optimization.
- The platform shows significant potential for the efficient discovery, development, and manufacture of polymeric nanoparticles.
