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Synthesis and characterization of unsaturated polyesters for use in multi-vesiculated particles (MVPs)

Thesis (MSc (Chemistry and Polymer Science))--University of Stellenbosch, 2010.

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Main Author: Simpson, Jaylin Mitch
Other Authors: Mallon, P. E.
Format: Thesis
Language:en_ZA
Published: Stellenbosch : University of Stellenbosch 2010
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access_status_str Open Access
author Simpson, Jaylin Mitch
author2 Mallon, P. E.
author_browse Mallon, P. E.
Simpson, Jaylin Mitch
author_facet Mallon, P. E.
Simpson, Jaylin Mitch
author_sort Simpson, Jaylin Mitch
collection Thesis
dc_rights_str_mv University of Stellenbosch
description Thesis (MSc (Chemistry and Polymer Science))--University of Stellenbosch, 2010.
format Thesis
id oai:scholar.sun.ac.za:10019.1/5177
institution Stellenbosch University (South Africa)
language en_ZA
last_indexed 2026-06-10T12:41:40.401Z
license_str Other — see source repository
provenance_str_mv Harvested via OAI-PMH from SUNScholar — Stellenbosch University Repository
publishDate 2010
publishDateRange 2010
publishDateSort 2010
publisher Stellenbosch : University of Stellenbosch
publisherStr Stellenbosch : University of Stellenbosch
record_format dspace
source_str SUNScholar — Stellenbosch University Repository
spelling oai:scholar.sun.ac.za:10019.1/5177 Synthesis and characterization of unsaturated polyesters for use in multi-vesiculated particles (MVPs) Simpson, Jaylin Mitch Mallon, P. E. McLeary, J. B. University of Stellenbosch. Faculty of Science. Dept. of Chemistry and Polymer Science. Polyesters -- Synthesis Multivesiculated particles Polycondensation process Dissertations -- Polymer science Theses -- Polymer science Chemistry and Polymer Science Thesis (MSc (Chemistry and Polymer Science))--University of Stellenbosch, 2010. ENGLISH ABSTRACT: Unsaturated polyesters resins (UPRs) of maleic anhydride (MA), phthalic anhydride (PA) and propylene glycol (PG) were synthesized using the fusion polycondensation process for use in Multi-vesiculated Particles (MVPs). The UPRs were synthesized using different MA:PA mole ratios and process parameters, including heating rates, agitation speed, exotherm rate and maximum processing temperature. Design of Experiments (DoE) software (Design Expert 7) was employed to find the optimum experimental space, i.e. least amount of experiments, but covering all the factors. The variations in the formulation and process parameters had a significant effect on the molecular structure and physical properties of the UPRs. The molecular structure and physical properties of the UPRs was successfully determined using various techniques including viscometry, acid-base titration, Proton Nuclear Magnetic Resonance (1H NMR) spectroscopy, Size-Exclusion Chromatography (SEC), Fourier Transform Infrared (FTIR) spectroscopy and Differential Scanning Calorimetry (DSC). Furthermore, the carboxyl and hydroxyl end-group concentrations of the UPRs were determined by derivatization of the groups with trichloroacetyl isocyanate (TAI) and analysis by 1H NMR. As a second part of the study, the effect of the above-mentioned monomer ratio and process factors of the UPRs, on the properties of the MVPs (produced from the UPRs), was investigated. Results showed that these factors had a significant effect on the particle size and degree of vesiculation of the MVPs. The degree of vesiculation of the MVPs was determined by Scanning Electron Microscopy (SEM). Attempts were also made to determine the relative hardness of the MVPs by AFM and microhardness testing to determine a relationship with UPRs properties (e.g. molecular weight, degree of unsaturation and chain branching). These techniques were however found to be unsuitable due to the physical nature of the MVPs. AFRIKAANSE OPSOMMING: Onversadigde poliësters (OPs) van maleïensuuranhidried (MA), fataalsuuranhidried (PA) en propileen glikol (PD) is berei deur die fusie polikondensasie-proses vir gebruik in multi-vesikulerende partikels (MVPs). Die OPs is berei deur gebruik te maak van verskillende MA:PA molverhoudings en reaksie faktore wat verhittingstempo‟s, roerspoed, eksoterm tempo en maksimum reaksie temperatuur, insluit. As gevolg van die groot hoeveelheid faktore is eksperimentontwerp sagteware (Design Expert 7) gebruik om die aantal eksperimente te verminder, maar ook waardevolle afleidings van die data te maak. Die verskille in die formulasie en reaksie faktore het „n merkwaardige effek op die molekulêre struktuur en fisiese eienskappe van die OPs gehad. Hierdie eienskappe is bepaal m.b.v. verskeie tegnieke, naamlik viskometrie, suur-basis titrasie, Proton Kern-Magnetiese Resonansie (1H KMR) spektroskopie, Grootte-Uitsluitings-Chromatografie (SEC), Fourier Transform Infrarooi (FTIR) spektroskopie en Differensiële Skandeerings Kalorimetrie (DSC). Die hidroksiel en karboksielgroep konsentrasies van die OPs is bepaal deur hul reaksie met trichloroasetiel-isosianaat (TAI) gevolg deur 1H KMR analise. In die tweede deel van hierdie studie is die invloed van bogenoemde faktore op die eienskappe van die MVPs ondersoek. Die resultate het getoon dat hierdie faktore „n merkwaardige effek op die partikel grootte en graad van “vesiculation” van die MVPs gehad het. Die graad van “vesiculation” van die MVPs is bepaal met behulp van Skandeer Elektron Mikroskopie (SEM). Pogings is ook gemaak om die relatiewe hardheid van die MVPs te bepaal deur middel van AFM en Mikro-hardheid toetsing. Dit is gedoen om die verhouding van die OPs eienskappe (molekulêre gewig, graad van onversadigheid en sy-kettings) vas te stel. Hierdie tegnieke is egter ongeskik bevind as gevolg van die inherente fisiese aard van die OPs. 2010-11-24T14:28:41Z 2010-12-15T10:18:25Z 2010-11-24T14:28:41Z 2010-12-15T10:18:25Z 2010-12 Thesis http://hdl.handle.net/10019.1/5177 en_ZA University of Stellenbosch application/pdf Stellenbosch : University of Stellenbosch
spellingShingle Polyesters -- Synthesis
Multivesiculated particles
Polycondensation process
Dissertations -- Polymer science
Theses -- Polymer science
Chemistry and Polymer Science
Simpson, Jaylin Mitch
Synthesis and characterization of unsaturated polyesters for use in multi-vesiculated particles (MVPs)
title Synthesis and characterization of unsaturated polyesters for use in multi-vesiculated particles (MVPs)
title_full Synthesis and characterization of unsaturated polyesters for use in multi-vesiculated particles (MVPs)
title_fullStr Synthesis and characterization of unsaturated polyesters for use in multi-vesiculated particles (MVPs)
title_full_unstemmed Synthesis and characterization of unsaturated polyesters for use in multi-vesiculated particles (MVPs)
title_short Synthesis and characterization of unsaturated polyesters for use in multi-vesiculated particles (MVPs)
title_sort synthesis and characterization of unsaturated polyesters for use in multi vesiculated particles mvps
topic Polyesters -- Synthesis
Multivesiculated particles
Polycondensation process
Dissertations -- Polymer science
Theses -- Polymer science
Chemistry and Polymer Science
url http://hdl.handle.net/10019.1/5177
work_keys_str_mv AT simpsonjaylinmitch synthesisandcharacterizationofunsaturatedpolyestersforuseinmultivesiculatedparticlesmvps