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1 Department of Chemical and Biochemical Engineering, Technical University of Denmark 2 The Danish Polymer Centre, Department of Chemical and Biochemical Engineering, Technical University of Denmark 3 Center for Energy Resources Engineering, Center, Technical University of Denmark 4 Department of Micro- and Nanotechnology, Technical University of Denmark 5 Centre for oil and gas – DTU, Center, Technical University of Denmark
Cured poly(dimethyl siloxane) microspheres are prepared by an emulsion polymerization reaction of silicone droplets in a continuous aqueous phase. The commonly used PDMS elastomer, Sylgard 184 from Dow Corning, is used as the dispersed phase. PDMS is polymerized and cross-linked by reacting vinyl end-terminated poly(dimethyl siloxane) oligomers with dimethylmethylhydrogen siloxane cross-linkers via the hydrosilylation reaction using platinum catalyst and heat. Weight ratios of 10:1, 20:1, and 25:1 of the PDMS mixtures are used and emulsified in water using two water-soluble surfactants as stabilizers (sodium dodecyl sulphate and polyvinylalcohol). The temperature is subsequently increased to accelerate the rate of cross-linking and prevent the prepolymer droplets from coalescing. The particle size distribution of cured PDMS microspheres is determined by Mastersizer (laser diffraction). Finally, cured PDMS microspheres are coated with poly(methyl methacrylate) using a chemical process (solvent evaporation technique). Three solvents are used in three different experiments: dichloromethane, tetrahydrofuran, and acetone. The composition and morphology of the cured PDMS microspheres and PMMA coated cured PDMS microspheres are characterized by differential scanning calorimetry, Fourier transform infrared spectroscopy in attenuated-total-reflection mode, optical microscopy, and thermogravimetric analysis. Curing profiles of PDMS elastomer with different ratios between the silicone elastomer base and the silicone elastomer curing agent are obtained. The reactivity of cured PDMS microspheres and PMMA coated cured PDMS microspheres are measured by rheology to evaluate the efficiency of the PMMA coating. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
Macromolecular Materials and Engineering, 2014, Vol 299, Issue 6, p. 729-738
emulsion polymerization; particle size distribution; PDMS microspheres; PMMA coatings; rheology; Acetone; Coatings; Crosslinking; Curing; Dichloromethane; Differential scanning calorimetry; Drops; Elasticity; Elastomers; Emulsification; Emulsion polymerization; Esters; Flocculation; Fourier transform infrared spectroscopy; Hydrosilylation; Microchannels; Microspheres; Particle size analysis; Plastics; Rheology; Thermogravimetric analysis; Attenuated-total-reflection; Hydrosilylation reaction; Laser diffractions; Pmma coatings; Silicone elastomers; Sodium dodecyl sulphate; Solvent evaporation techniques; Water-soluble surfactants; Silicones
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