A scalable method for the synthesis of polyethylene terephthalamide microcapsules grafted with polyacrylic acid to enable pH responsiveness has been developed. Microcapsules were produced by interfacial polymerisation of an oil-in-water emulsion in a 2 L batch reactor and subsequently circulated through an external loop reactor for UV irradiative surface grafting. Ungrafted microcapsule samples yielded 1.0 - 1.2 g desiccated capsules per experiment. Initial production trials were subject to severe agglomeration, observed during dialysis of the microcapsules with 30 % (v/v) ethanol solution. Lowering of the terephthaloyl dichloride monomer concentration, to 0.2 mol L⁻¹ in the chloroform / cyclohexane (3 : 1) organic solution, alleviated this unwanted agglomeration. Laser diffraction particle size analysis revealed microcapsules were produced with a 51 µm average diameter. A purpose built external loop irradiation reactor was used to facilitate graft polymerisation of acrylic acid on the microcapsules, using 254 nm UV light at 19 mW cm⁻². Characterisation of the external loop flow regime showed a mild deviation from ideal plug flow, with a vessel dispersion number of 0.014 and a Reynolds number of 1310. Confirmation of monomer polymerisation was ascertained by back titration and Fourier transform infrared spectroscopy. No distinction between homopolymer and grafted polyacrylic acid could be made by these characterisation methods. A Taguchi analysis on variables influencing grafting revealed high temperature to contribute most significantly to graft yield, followed by a long irradiation period. The development of a packed column pulse response method for testing pH response showed a high repeatability. However, release profile testing of a microcapsule slurry with an observed graft yield of 1.13 mmol g⁻¹ did not provide a definitive pH-based release of mPEG 5000 or PEGylated TAMRA dye. Determination of acrylic acid polymerisation kinetics following UV irradiation of the microcapsules is required for future optimisation of a functional graft yield.
| Identifer | oai:union.ndltd.org:canterbury.ac.nz/oai:ir.canterbury.ac.nz:10092/1988 |
| Date | January 2008 |
| Creators | Kelton, William James |
| Publisher | University of Canterbury. Chemical and Process Engineering |
| Source Sets | University of Canterbury |
| Language | English |
| Detected Language | English |
| Type | Electronic thesis or dissertation, Text |
| Rights | Copyright William James Kelton, http://library.canterbury.ac.nz/thesis/etheses_copyright.shtml |
| Relation | NZCU |
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