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Drying, Film Formation and Open Time of Aqueous Polymer Dispersions an Investigation of Different Aspects by Rheometry and Inverse-Micro-Raman-Spectroscopy (IMRS)

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Drying, Film Formation and Open Time of Aqueous Polymer Dispersions an Investigation of Different Aspects by Rheometry and Inverse-Micro-Raman-Spectroscopy (IMRS) Imke Ludwig Drying, Film Formation and Open Time of Aqueous Polymer Dispersions An Investigation of Different Aspects by Rheometry and Inverse-Micro-Raman-Spectroscopy (IMRS) Drying, Film Formation and Open Time of Aqueous Polymer Dispersions An Investigation of Different Aspects by Rheometry and Inverse-Micro-Raman-Spectroscopy (IMRS) by Imke Ludwig Dissertation, Universität Karlsruhe (TH) Fakultät für Chemieingenieurwesen und Verfahrenstechnik, 2008 Impressum Universitätsverlag Karlsruhe c/o Universitätsbibliothek Straße am Forum 2 D-76131 Karlsruhe www.uvka.de Dieses Werk ist unter folgender Creative Commons-Lizenz lizenziert: http://creativecommons.org/licenses/by-nc-nd/2.0/de/ Universitätsverlag Karlsruhe 2008 Print on Demand ISBN: 978-3-86644-284-9 Drying, Film Formation and Open Time of Aqueous Polymer Dispersions -An Investigation of Different Aspects by Rheometry and Inverse-Micro-Raman-Spectroscopy (IMRS)- Zur Erlangung des akademischen Grades eines Doktors der Ingenieurwissenschaften (Dr.-Ing.) der Fakultät für Chemieingenieurwesen und Verfahrenstechnik der Universität Fridericiana Karlsruhe (Technische Hochschule) genehmigte Dissertation von Dipl.-Ing. Imke Ludwig geboren in Berlin-Wilmersdorf Tag des Kolloquiums: 8. Juli 2008 Referent: Prof. Dr.-Ing. Matthias Kind Korreferent: Prof. Dr. Norbert Willenbacher I Preface This thesis is the final work of my Ph.D. study at the Institute of Thermal Process Engineering at the University of Karlsruhe (TH), which has been made from fall 2002 until spring 2007. The project is the result of a longlasting cooperation with the Rhodia Research and Technology Centers in Aubervilliers and Lyon (France): I started working on the new project entitled “Drying and Film Formation of Aqueous Dispersion Formulations” in October of 2002. It required the use of the measurement technique of Inverse-Micro-Raman- Spectroscopy (IMRS) that was brought to the institute by Wilhelm Schabel shortly before. By the success of the IMRS-technique, the research group grew to a size of ~4-5 PhD students. What I present in the following chapters is the result of the work that I did together with students, technicians and other colleagues. I like to use this to thank all the people who contributed to this work, and my colleagues who created a pleasant and inspiring atmosphere to work in. I very much enjoyed working in Karlsruhe and in the Raman group. First of all, I thank Prof. Dr.-Ing. Matthias Kind. He has been a very stimulating advisor who gave me a lot of freedom. It was very motivating that he was as excited about the research as I was. I am very grateful for setting up the long-lasting cooperation with Rhodia (France), that enabled this very interesting project. Besides, he gave me the opportunity to participate regularly in international conferences. I would also like to thank Prof. Dr. Norbert Willenbacher for his interest in this project and for serving as a second censor for this work. During my Ph.D. work, Dr.-Ing. Wilhelm Schabel became a second Ph.D. advisor for me. I would like to thank him for the many discussions and important suggestions concerning the progress of my work. I enjoyed being the advisor of a number of students: I like to thank Peter Demarez and Jason Chan, for the excellent work during their diploma theses and also Özgül Gediekli and Karsten Pabst for their hard work during their seminar theses. Natalia Bylik, Markus Wetzel and Steffen Waglöhner must be mentioned because of the great job they did to obtain experimental results when working as a student researcher. Thank you for the good collaboration and the excellent results that were essential for the success of this work. Many other colleagues in Karlsruhe contributed to this work with help, critical questions, stimulating discussions, and being friends during and after work. I would like to mention Gisela Schimana, Prof. Dr.-Ing. Holger Martin, Prof. Dr.-Ing. Ernst-Ulrich Schlünder, Prof. Dr.-Ing. Volker Gnielinski and Lothar Eckert who must be named in connection with the day- to-day work at the institute. The support from several technicians in our institute has been indispensable for getting results. Especially I want to mention Patrick Ferlin, Jean-Christophe Castaing and Philippe Olier of Rhodia (France) and would like to say thank you for the scientific discussions in Paris, Lyon and in Karlsruhe. Most notably, I like to thank my parents for always following and supporting my work with great interest. II Table of Contents III Table of Contents Symbols and Abbreviations VII 1 Introduction........................................................................................................... 1 1.1 Introduction.................................................................................................... 1 1.2 State of the Art................................................................................................ 3 1.3 Aim of this Work/Investigated Aspects.......................................................... 8 2 Aqueous Polymer Dispersions ........................................................................... 11 2.1 Latex Dispersions......................................................................................... 11 2.1.1 Composition.............................................................................................. 11 2.1.2 Investigated Dispersions........................................................................... 12 2.2 Polyurethane (PU) Emulsions..................................................................... 15 2.2.1 Composition.............................................................................................. 15 2.2.2 Emulsion Preparation................................................................................ 15 3 Rheology of Polymer Dispersions...................................................................... 17 3.1 Rheological Characteristics of Concentrated Polymer Dispersions.......... 17 3.1.1 Viscoelastic Properties.............................................................................. 18 3.1.2 Liquid-Solid Transition and Gelation....................................................... 19 3.1.3 The Cox-Merz Rule................................................................................... 20 3.1.4 Theoretical Description of the Viscosity Function................................... 20 3.1.5 Mean Particle Separation and Polymer Volume Fraction ........................ 24 4 Mechanism of Film Formation .......................................................................... 27 4.1 Latex Dispersions: Film Formation by Physical Driving Forces.............. 27 4.1.1 The Different Stages of Film Formation................................................... 27 4.1.2 The Driving Forces for Film Formation ................................................... 29 4.2 PU Emulsions: Film Formation by Chemical Crosslinking...................... 29 4.3 Horizontal Inhomogeneous Drying ............................................................ 31 5 Local Concentration Measurements (by IMRS).............................................. 33 5.1 Experimental Setup...................................................................................... 33 5.1.1 Air Conditioning....................................................................................... 33 5.1.2 Inverse-Micro-Raman-Spectrometer (IMRS)........................................... 34 5.2 Spectra Calibration ...................................................................................... 35 5.2.1 Raman Spectra of Relevant Components ................................................. 35 5.2.2 Concentration Measurements ................................................................... 38 5.2.3 Spectra Evaluation .................................................................................... 40 IV Table of Contents 5.3 Signal Intensity Loss by Scattering in Polymer Dispersions ..................... 42 5.3.1 Particle Size Effect.................................................................................... 45 5.3.2 Solid Content of the Dispersion................................................................ 48 5.3.3 Appraisal of these Effects on the Quantitative Data Evaluation .............. 48 6 Model Calculations ............................................................................................. 53 6.1 Film Leveling ............................................................................................... 53 6.2 Film Drying.................................................................................................. 55 6.2.1 Mass Transport in the Gas Phase (Constant-Rate-Model) ....................... 56 6.2.2 Water Sorption and Phase Equilibrium .................................................... 56 6.2.3 Water Diffusion in the Film...................................................................... 57 6.2.4 Mathematical Description of Drying (Vertical Direction) ....................... 58 6.2.5 Mathematical Description of Drying (Horizontal Direction) ................... 61 7 Results and Discussion........................................................................................ 65 7.1 Rheology of Aqueous Latex Dispersions .................................................... 65 7.1.1 Rheological Investigation of the Concentrated Dispersions..................... 65 7.1.2 Rheological Properties as a Function of the Water Content X................. 68 7.1.3 Viscosity Functions..................................................................................
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