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Quest for Thermoresponsive Block Copolymer Nanoparticles with Liquid-Crystalline Surfactant Cores.

ABSTRACT: This work reports on the preparation and characterization of anisotropic composition nanoparticles based on the electrostatic binding of dodecyltrimethylammonium surfactant to poly(acrylic acid) blocks of diblock copolymers with poly(ethylene oxide) (PEO) and poly(N-isopropyl acrylamide) (PNIPAm). These nanoparticles form kinetically stable dispersions and display liquid-crystalline cores with a micellar cubic structure, as determined by small-angle X-ray scattering. Mixtures with different proportions of the two block copolymers and stoichiometric amounts of C₁₂TA⁺ were prepared and their behavior was compared with that of the parent nanoparticles. Upon heating, dilute dispersions (0.01 and 0.1 wt %) analyzed by dynamic light scattering display a slight decrease in the hydrodynamic radius, consistent with the dehydration of PNIPAm and mixed PNIPAm-PEO blocks at the shell. At higher concentrations, 2 wt %, the nanoparticles with pure PNIPAm shell undergo macroscopic phase separation above 32 °C. Nanoparticles with a pure PEO shell do not display temperature sensitivity. For the mixtures, no visual change is observed, but the dynamic light scattering results evidence the formation of clusters, whose size and reversibility depend on the PEO/PNIPAm proportion. This indicates the formation of mixed nanoparticles containing both PEO and PNIPAm blocks. Nuclear Overhauser enhancement spectroscopy NMR analyses of the mixtures do not show the correlation peak expected for PEO and PNIPAm blocks in close proximity, suggesting their segregation at the nanoparticle shell. On the basis of these results, we discuss the possibilities of the neutral blocks distribution on the shell of mixed nanoparticles. Overall, we have confirmed that these nanoparticles may display a temperature-controlled reversible aggregation while preserving their internal liquid-crystalline structures.

SUBMITTER: Carneiro NM

PROVIDER: S-EPMC6644550 | biostudies-literature | 2017 Sep

REPOSITORIES: biostudies-literature

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Quest for Thermoresponsive Block Copolymer Nanoparticles with Liquid-Crystalline Surfactant Cores.

Carneiro Nathalia M NM Percebom Ana M AM Loh Watson W

ACS omega 20170906 9

This work reports on the preparation and characterization of anisotropic composition nanoparticles based on the electrostatic binding of dodecyltrimethylammonium surfactant to poly(acrylic acid) blocks of diblock copolymers with poly(ethylene oxide) (PEO) and poly(<i>N</i>-isopropyl acrylamide) (PNIPAm). These nanoparticles form kinetically stable dispersions and display liquid-crystalline cores with a micellar cubic structure, as determined by small-angle X-ray scattering. Mixtures with differe ...[more]

PMID: 31457819

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Project description:Well-defined sterically stabilized diblock copolymer nanoparticles of 29 nm diameter are prepared by RAFT aqueous emulsion polymerization of methyl methacrylate using a dithiobenzoate-capped poly(glycerol monomethacrylate) precursor. These nanoparticles are evaluated as a dispersant for the preparation of organic crystalline microparticles via ball milling. This is exemplified for azoxystrobin, which is a broad-spectrum fungicide that is widely used to protect various food crops. Laser diffraction and optical microscopy studies indicate the formation of azoxystrobin microparticles of approximately 2 μm diameter after ball milling for 10 min at 400 rpm. Nanoparticle adsorption at the surface of these azoxystrobin microparticles is confirmed by electron microscopy studies. The extent of nanoparticle adsorption on the azoxystrobin microparticles can be quantified using a supernatant assay based on solution densitometry. This technique indicates an adsorbed amount of approximately 5.5 mg m-2, which is sufficient to significantly reduce the negative zeta potential exhibited by azoxystrobin. Moreover, this adsorbed amount appears to be essentially independent of the nature of the core-forming block, with similar data being obtained for both poly(methyl methacrylate)- and poly(2,2,2-trifluoroethyl methacrylate)-based nanoparticles. Finally, X-ray photoelectron spectroscopy studies confirm attenuation of the underlying N1s signal arising from the azoxystrobin microparticles by the former adsorbed nanoparticles, suggesting a fractional surface coverage of approximately 0.24. This value is consistent with a theoretical surface coverage of 0.25 calculated from the adsorption isotherm data. Overall, this study suggests that sterically stabilized diblock copolymer nanoparticles may offer a useful alternative approach to traditional soluble copolymer dispersants for the preparation of suspension concentrates affecting the context of agrochemical applications.

Dataset Information

Quest for Thermoresponsive Block Copolymer Nanoparticles with Liquid-Crystalline Surfactant Cores.

Publications

Quest for Thermoresponsive Block Copolymer Nanoparticles with Liquid-Crystalline Surfactant Cores.

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