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Small and Wide Angle X-Ray Scattering Studies of Biological Macromolecules in Solution

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Time-Resolved Small-Angle X-ray Scattering Studies during Aqueous Emulsion Polymerization.

Adam Czajka¹, Steven P Armes¹

¹Department of Chemistry, University of Sheffield, Dainton Building, Brook Hill, Sheffield S3 7HF, United Kingdom.

Journal of the American Chemical Society

|January 14, 2021

Summary

This summary is machine-generated.

This study used time-resolved small-angle X-ray scattering (SAXS) to investigate the emulsion polymerization of 2,2,2-trifluoroethyl methacrylate (TFEMA). Researchers observed distinct differences in particle formation between surfactant-free and sodium dodecyl sulfate (SDS) formulations.

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Structural Studies of Macromolecules in Solution using Small Angle X-Ray Scattering

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Published on: November 5, 2018

Area of Science:

Polymer Chemistry
Materials Science
Physical Chemistry

Background:

Aqueous emulsion polymerization is a key industrial process for producing polymer latexes.
Understanding polymerization kinetics and particle formation is crucial for controlling material properties.
2,2,2-trifluoroethyl methacrylate (TFEMA) offers advantages in X-ray scattering contrast for in situ studies.

Purpose of the Study:

To investigate the emulsion polymerization of TFEMA using time-resolved small-angle X-ray scattering (SAXS).
To monitor particle size evolution and polymerization kinetics in the presence and absence of sodium dodecyl sulfate (SDS).
To elucidate the mechanism of aqueous emulsion polymerization through in situ SAXS analysis.

Main Methods:

Persulfate-initiated aqueous emulsion polymerization of TFEMA at 60 °C.
Time-resolved small-angle X-ray scattering (SAXS) using a stirrable reaction cell.
Ex situ dynamic light scattering (DLS) and post-mortem SAXS for particle size analysis.
¹H NMR spectroscopy for conversion determination.
Hard sphere scattering model fitting for particle growth analysis.

Main Results:

Well-defined spherical latexes were formed, with volume-average diameters of 353 ± 9 nm (surfactant-free) and 68 ± 4 nm (SDS).
TFEMA conversions reached 99% (surfactant-free) and 93% (SDS) within 80 and 60 minutes, respectively.
In situ SAXS identified three main intervals during polymerization in the presence of SDS, consistent with other methods.
Nucleation occurred at approximately 6 minutes for both formulations.

Conclusions:

Significant differences in particle size and polymerization kinetics were observed between surfactant-free and SDS formulations.
In situ SAXS is a powerful tool for real-time monitoring of emulsion polymerization mechanisms.
The study provides valuable insights into the role of surfactants in TFEMA emulsion polymerization.