Strategic Aspects of the Incorporation of Acrylic Acid in Emulsion Polymers

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Strategic Aspects of the Incorporation of Acrylic Acid in Emulsion Polymers Strategic aspects of the incorporation of acrylic acid in emulsion polymers Citation for published version (APA): Slawinski, M. (1999). Strategic aspects of the incorporation of acrylic acid in emulsion polymers. Technische Universiteit Eindhoven. https://doi.org/10.6100/IR526315 DOI: 10.6100/IR526315 Document status and date: Published: 01/01/1999 Document Version: Publisher’s PDF, also known as Version of Record (includes final page, issue and volume numbers) Please check the document version of this publication: • A submitted manuscript is the version of the article upon submission and before peer-review. There can be important differences between the submitted version and the official published version of record. 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Link to publication General rights Copyright and moral rights for the publications made accessible in the public portal are retained by the authors and/or other copyright owners and it is a condition of accessing publications that users recognise and abide by the legal requirements associated with these rights. • Users may download and print one copy of any publication from the public portal for the purpose of private study or research. • You may not further distribute the material or use it for any profit-making activity or commercial gain • You may freely distribute the URL identifying the publication in the public portal. If the publication is distributed under the terms of Article 25fa of the Dutch Copyright Act, indicated by the “Taverne” license above, please follow below link for the End User Agreement: www.tue.nl/taverne Take down policy If you believe that this document breaches copyright please contact us at: [email protected] providing details and we will investigate your claim. Download date: 25. Sep. 2021 Strategie Aspects of the lncorporation of Acrylic Acid ·n Emulsion Polymers Marfine Slawinski Strategie Aspects of the Incorpora ti on of Acrylic Acid in Emulsion Polymers Martine Slawinski CJP-DATA LIBRARY TECHNISCHE UNIVERSITEIT EINDHOVEN Slawinski, Manine S!Tategic aspects ofthe incorporation ofacrylic acid in emulsion polymers I by Martine Slawinski. - Eindhoven : Technische Universiteit Eindhoven, 1999. Proefschrift. -ISBN 90-386-267 I -I NUGI 813 Trefwoorden: emulsie-polymerisatie Subject headings: emulsion polymerization Druk: Universiteitsdrukkerij Technische Universiteit Eindhoven Strategie Aspects ofthe Incorporation of Acrylic Acid in Emulsion Polymers PROEFSCHRIFT ter verkrijging van de graad van doctor aan de Technische Universiteit Eindhoven, op gezag van de Rector Magnificus, prof. Dr. M. Rem, voor een commissie aangewezen door het College voor Promoties in het openbaar te verdedigen op woensdag 20 oktober 1999 om 16.00 uur door Martine Slawinski geboren te Somain (Frankrijk) Dit proefschrift is goedgekeurd door de promotoren: prof. dr. ir. A. L. German en prof. dr. G. Riess Copromotor: dr. J. Meuldijk Les gens on/ des étoiles quine sant pas les mêmes. Pour les uns, qui voyagent, les étoiles sant des guides. Pour d'alllres el/es ne sant rien que de peti/es lumières. Pour d 'autres, qui sant savants, el/es sant des problèmes. ( .. ) Ma is taules ces étoiles /à se taisent. Toi, tu auras des étoiles comme personne n'en a .. ( .. ) Tu auras, toi, des étoiles qui saven/ rire! Antoine de Saint-Exupéry "Le Petit Prince" (1 946) Pour mon père ... SAMENVATTING Het doel van dit proefschrift was om de kennis te verbeteren omtrent inbouw van carbonzuurfunctionele monomeren in polymeren gemaakt in emulsie. Zodoende is de invloed van acrylzuur op het verloop van de emulsiecopolymerisatie met styreen en met styreen en butadieen onderzocht. De aandacht is voornamelijk gericht op de hoeveelheid carboxylgroepen die worden ingebouwd gedurende het proces. De invloed van de pH van het reactiemengsel op het verloop van de reactie en de inbouw van acrylzuur in de polymeerdeeltjes is onderzocht zowel aan de hand van ab-initia experimenten als met experimenten met een kiemlatex. Er zijn diverse analytische methoden ontwikkeld en toegepast om de carboxylgroepen in de latex te karakteriseren. Het is mogelijk gebleken de conductometrische titratie in waterig milieu van verdunde latexmonsters na dialyse te combineren met de potentiometrische titratie van de corresponderende opgeloste deeltjesfase in niet-waterige oplosmiddelen. Door middel van deze werkwijze kon de verdeling van polymeren met carboxylgroepen over de verschillende plaatsen in het reactiemengsel, dat wil zeggen begraven in de latexdeeltjes, aan het oppervlak ervan of in de waterfase, worden achterhaald. Voor de bepaling van de intermoleculaire chemische samenstellingsverdeling is gradiënt hoge druk vloeistof chromatografie ontwikkeld voor copolymeren van styreen en butadieen enerzijds en copolymeren van styreen en acrylzuur anderzijds. Er is aangetoond dat bij het gebruik van deze methode de invloed van molecuulmassa van de corresponderende solutie­ en emulsiecopolymeren op het chromatografische scheidingsproces de interpretatie van de resultaten emstig bemoeilijkt. De invloed van pH op de polymerisatiekinetiek van carbonzuurfunctionele monomeren in water is onderzocht met behulp van gepulseerde laser polymerisatie in combinatie met ' size exclusion chromatography' aan polymeren die gemodificeerd zijn door verestering van de carboxylgroepen. Voor dit deelonderzoek is methacrylzuur gebruikt bij verschillende pH-waarden en een constante ionensterkte. Het bleek dat de propagatiesnelheidsconstante van methacrylzuur hoog was onder zure condities, dat wil zeggen pH 2. De reactiesnelheidsconstante daalde vervolgens met toenemende pH en vertoonde een minimumwaarde bij een pH van 7. Dit gedrag is geëxtrapoleerd naar de emulsiepolymerisatie van styreen met acrylzuur als comonomeer. De invloed van zowel de pH als de hoeveelheid acrylzuur op enerzijds de propagatiesnelheidsconstante en anderzijds de chemische samenstelling van de gedurende het proces in de continue fase gevormde copolymeren is aangetoond. Echter, als gevolg van een lage verdelingscoëfficiënt tussen de organische en de waterfase heeft acrylzuur slechts een kleine invloed op de totale polymerisatiesnelheid. Dit gedrag werd ondersteund door afschatting van de gemiddelde propagatiesnelheidsconstante in de deeltjesfase. Emulsiepolymerisatie experimenten met styreen of met styreen en butadieen zijn uitgevoerd. Het gebruik van acrylzuur in de polymerisatiereceptuur, tezamen met de pH van het reactiemengsel, bleek een sterke invloed te hebben op zowel het deeltjesvorrningsproces als de effectiviteit van inbouw van de zuurgroepen. Relatief hoge acrylzuurconcentraties, alsmede een lage pH, resulteerden in een hoge concentratie latexdeeltjes en een relatief grote fractie van de carboxylgroepen ingebouwd in de polymeermoleculen die zich aan het oppervlak van de uiteindelijke latexdeeltjes bevinden. Kinetisch onderzoek aan emulsiepolymerisatiesystemen met een kiemlatex heeft geen duidelijkheid verschaft over de invloed van acrylzuur en de pH op de polymerisatiesnelheid per latexdeeltje in aanwezigheid van monomeerdruppels. Zowel ab-initia als experimenten met een kiemlatex hebben aangetoond dat acrylzuur voornamelijk wordt ingebouwd aan het oppervlak van de latexdeeltjes. Deze inbouw vindt bij voorkeur plaats gedurende de laatste fase van het emulsiepolymerisatieproces bij lage pH en bij een hoog specifiek oppervlak van de latexdeeltjes. De verkregen resultaten leverden een helderder beeld op van de optredende mechanismen in de produktie van gecarboxyleerde Iatices. Experimenten waarbij acrylzuur strategisch werd geïntroduceerd in de laatste fase van de emulsiepolymerisatiereactie bij lage pH resulteerden in een optimale inbouweffectiviteit van carboxylgroepen aan het oppervlak van de Iatexdeeltjes. RESUME Le but du travail entrepris est l'amélioration de nos connaissances concemant l'incorporation de monomères carboxyliques dans les polymères préparés suivant Ie procédé de polymérisation en émulsion. Le röle de l'acide acrylique durant sa copolymérisation en émulsion avec Ie styrène et avec un mélange de styrène et de butadiène a été étudié. La quantité de groupes carboxyliques incorporée dans les polymères formés au cours de la polymérisation a retenu une attention toute particulière. Le pH a été étudié en tant que paramètre principal des expériences conduites ab-initia ou en présence d'un latex semence. Des méthodes analytiques ont été développées afin de caractériser les produits de polymérisation contenant des fonctions carboxyliques. Le dosage des groupes acide a pu être effectué par conductimétrie pour les latex dilués et par pH-métrie pour les polymères en solution dans un solvant organique. De cette manière, la distribution des groupes carboxyliques entre l'intérieur des particules de latex, leur surface ainsi que la phase continue a pu être déterminée. La séparation chromatographique des copolymères par gradient de solvants permet d'établir leur distribution intermoléculaire de compositions chimiques. La méthode a été développée avec succès pour Jes copolymères de styrène et butadiène ainsi que les copolymères de styrène et d'acide acrylique. Cependant il a été noté que la séparation était également fonction de la masse moléculaire
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