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Inhibiting the Thermal Gelation of Copolymer Stabilized Nonaqueous Dispersions and the Synthesis of Full Color PMMA Particles

Belsey, Kate E., Topping, Claire, Farrand, Louise D., Holder, Simon J. (2016) Inhibiting the Thermal Gelation of Copolymer Stabilized Nonaqueous Dispersions and the Synthesis of Full Color PMMA Particles. Langmuir, 32 (11). pp. 2556-2566. ISSN 0743-7463. E-ISSN 1520-5827. (doi:10.1021/acs.langmuir.6b00063) (KAR id:54590)

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Abstract

Polymeric particle dispersions have numerous potential applications; currently one of the most relevant is their use as inks in electrophoretic displays. These colloidal particles are synthesized from the appropriate monomer using nonaqueous dispersion (NAD) polymerization in a nonpolar solvent, which requires a stabilizer to control particle size and morphology. We have previously reported the facile synthesis of poly(methyl methacrylate)-block-poly(octadecyl acrylate) (PMMA-b-PODA) by atom transfer radical polymerization (ATRP), and its use in the NAD polymerization of MMA in hexane/dodecane solvent mixtures. Here we report the synthesis of monodisperse PMMA particles in dodecane following a standard “industrial” procedure using these PMMA-b-PODA stabilizers. However, it was observed that the particle suspensions solidified when they were left at temperatures below ?18 °C yet redispersed upon being heated. Differential scanning calorimetry, dynamic light scattering, and rheological studies demonstrated that this thermoresponsive behavior was due to a liquid–gel transition occurring at 17.5 °C as a consequence of the upper critical solution temperature of PODA in dodecane being traversed. Consequently, new copolymers were synthesized by ATRP with an ethylhexyl acrylate (EHA) co-monomer incorporated into the lyophilic (dodecane compatible) block. Dispersions stabilized by these PMMA-b-P(ODA-co-EHA) polymers with high EHA contents exhibited lower gelation temperatures because of the greater solvent compatibility with dodecane. The use of a PMMA65-b-(ODA10-co-EHA45) copolymer stabilizer (with the highest EHA content) gave PMMA dispersions that showed no gelation down to 4 °C and monodisperse cross-linked PMMA particles containing organic dyes (cyan, magenta, red, and black) giving colored particles across the size range of approximately 100–1300 nm.

Item Type: Article
DOI/Identification number: 10.1021/acs.langmuir.6b00063
Subjects: Q Science > QD Chemistry > QD473 Physical properties in relation to structure
Divisions: Faculties > Sciences > School of Physical Sciences > Functional Materials Group
Depositing User: Simon Holder
Date Deposited: 22 Mar 2016 11:08 UTC
Last Modified: 01 Aug 2019 10:40 UTC
Resource URI: https://kar.kent.ac.uk/id/eprint/54590 (The current URI for this page, for reference purposes)
Holder, Simon J.: https://orcid.org/0000-0001-8977-9257
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