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Block Copolymer Nanoparticles are Effective Dispersants for Micrometer-Sized Organic Crystalline Particles.

ABSTRACT: 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.

SUBMITTER: Chan DHH

PROVIDER: S-EPMC8289232 | biostudies-literature |

REPOSITORIES: biostudies-literature

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Project description:A series of linear cationic diblock copolymer nanoparticles are prepared by polymerization-induced self-assembly (PISA) via reversible addition-fragmentation chain transfer (RAFT) aqueous dispersion polymerization of 2-hydroxypropyl methacrylate (HPMA) using a binary mixture of non-ionic and cationic macromolecular RAFT agents, namely poly(ethylene oxide) (PEO113, Mn = 4400 g mol-1; Mw/Mn = 1.08) and poly([2-(methacryloyloxy)ethyl]trimethylammonium chloride) (PQDMA125, Mn = 31?800 g mol-1, Mw/Mn = 1.19). A detailed phase diagram was constructed to determine the maximum amount of PQDMA125 stabilizer block that could be incorporated while still allowing access to a pure worm copolymer morphology. Aqueous electrophoresis studies indicated that zeta potentials of +35 mV could be achieved for such cationic worms over a wide pH range. Core cross-linked worms were prepared via statistical copolymerization of glycidyl methacrylate (GlyMA) with HPMA using a slightly modified PISA formulation, followed by reacting the epoxy groups of the GlyMA residues located within the worm cores with 3-aminopropyl triethoxysilane (APTES), and concomitant hydrolysis/condensation of the pendent silanol groups with the secondary alcohol on the HPMA residues. TEM and DLS studies confirmed that such core cross-linked cationic worms remained colloidally stable when challenged with either excess methanol or a cationic surfactant. These cross-linked cationic worms are shown to be much more effective bridging flocculants for 1.0 ?m silica particles at pH 9 than the corresponding linear cationic worms (and also various commercial high molecular weight water-soluble polymers.). Laser diffraction studies indicated silica aggregates of around 25-28 ?m diameter when using the former worms but only 3-5 ?m diameter when employing the latter worms. Moreover, SEM studies confirmed that the cross-linked worms remained intact after their adsorption onto the silica particles, whereas the much more delicate linear worms underwent fragmentation under the same conditions. Similar results were obtained with 4 ?m silica particles.

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Block Copolymer Nanoparticles are Effective Dispersants for Micrometer-Sized Organic Crystalline Particles.

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