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Characterization and Surface Modification of Rubber From Characterization and Surface Modification of Rubber from Recycled Tires Thèse Huan Liang Doctorat en Chimie Philosophiae doctor (Ph. D.) Québec, Canada © Huan Liang, 2015 Characterization and Surface Modification of Rubber from Recycled Tires Thèse Huan Liang Sous la direction de : Josée Brisson, directrice de recherche Résumé Les pneus en fin de cycle de vie soulèvent de graves problèmes environnementaux. Ils doivent être éliminés ou recyclés. En raison de leur structure réticulée, les pneus ne fondent pas ni ne se dissolvent. Ils sont généralement broyés en poudre (caoutchouc de pneu broyé, abrévié GTR). Ensuite, ces poudres sont mélangées avec une matrice (asphalte ou polymère thermoplastique) pour réutilisation. L'industrie du recyclage se heurte à deux problèmes principaux. En premier lieu, le contrôle de technique qualité est difficile à cause du manque de solubilité de la poudre et de moyens limités pour ces petites industries. Il est nécessaire de trouver des méthodes rapides et à faible coût pour améliorer la caractérisation des GTR. Dans le présent travail, nous avons mis l'accent sur l'utilisation de ces deux techniques et sur la spectrométrie de fluorescence-X (XRF), comme il y a des rapports dans la littérature démontrant que ceux-ci peuvent être utilisés, respectivement, pour déterminer la densité de réticulation, la composition en monomères et la composition élémentaire. Un deuxième problème est la faible adhérence entre la plupart des polymères et les GTR. Ceci résulte en un manque de résistance mécanique et une tendance à l'effritement des pièces fabriquées. Certaines études se concentrent sur l'ajout de monomère et d'initiateur au GTR, afin de faire une polymérisation in-situ de chaînes greffées sur la surface. Cependant, le poids moléculaire des greffons est inconnu et il est impossible de vérifier si celui-ci est supérieur au poids moléculaire d'enchevêtrement des chaînes. Des réactions photochimiques ont été utilisées pour greffer des chaînes polymériques terminées par un groupement thiol de poids moléculaire connu en utilisant les liaisons doubles présentes à la surface de GTR. La spectrométrie de photoélectrons induits par rayons X (XPS) et la spectroscopie infrarouge à transformée de Fourier (FTIR) ont été utilisées pour détecter les changements de surface et vérifier si le greffage a bien eu lieu. Finalement, la mesure des propriétés mécaniques a été utilisée pour évaluer l’effet du greffage avec les échantillons de GTR greffé mélangés à du polystyrène commercial. iii Abstract End of life tires raise severe environmental problems and must be disposed of or recycled. Due to their cross-linked structure, they do not melt or dissolve, and are usually ground into a powder (ground tire rubber or GTR) and mixed with a matrix (asphalt or a thermoplastic polymer) for reuse. The recycling industry encounters two main problems. First, quality control is difficult due to the lack of solubility of the powder and to the limited technical means of these small industries. Rapid and low-cost methods are needed to improve characterization of GTR. This work focused on the use of these two techniques and of X-ray fluorescence spectrometry (XRF), as there are reports in the literature showing than these may be used, respectively, to determine cross-link density, monomer and elemental composition. The second problem is the poor adhesion between most polymers and GTR, resulting in parts that lack mechanical strength and tend to crumble. Some studies focus on adding monomer and initiator to GTR and doing in-situ polymerization of graft chains onto the surface. However, molecular weight of grafts is unknown and it is not possible to verify if the molecular weight is above the chain entanglement molecular weight. Photochemical reactions were used to graft thiol-terminated polymer chains of known molecular weight by using free carbon double bonds that exist on the GTR surface. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) were used to detect the surface changes and graft degree. Mechanical properties measurement was used to monitor the treated samples blends with polystyrene matrix. iv Table of Contents Résumé ................................................................................................................................. iii Abstract ................................................................................................................................. iv Table of Contents .................................................................................................................. v List of Tables ..................................................................................................................... viii List of Figures ....................................................................................................................... ix Abbreviations ........................................................................................................................ x Symbols ................................................................................................................................. xi Acknowledgments ............................................................................................................. xiii Foreword .............................................................................................................................. xv Chapter 1: Introduction ....................................................................................................... 1 1.1 End of life tires .............................................................................................................. 1 1.2 The problem of end of life tire disposal ........................................................................ 5 1.3 Tire recycling ................................................................................................................ 5 1.3.1 Crumb rubber modified asphalt .............................................................................. 6 1.3.2 Pyrolysis ................................................................................................................. 7 1.3.3 Crumb rubber modification .................................................................................... 8 1.4 Thermoplastic recycling using crumb rubber ............................................................. 12 1.5 Quality control of crumb rubber ................................................................................. 15 1.5.1 Cross-linking density ............................................................................................ 15 1.5.2 Monomer composition .......................................................................................... 18 1.5.3 Carbon Black ........................................................................................................ 20 1.5.4 Inorganics ............................................................................................................. 20 1.6 Project Objectives ....................................................................................................... 21 Chapter 2: EPDM Recycled Rubber Powder Characterization: Thermal and Thermogravimetric Analysis ............................................................................................. 25 Résumé .............................................................................................................................. 26 Abstract ............................................................................................................................. 27 2.1 Introduction ................................................................................................................. 28 2.2 Experimental ............................................................................................................... 30 2.2.1 Preparation of Rubber Standards .......................................................................... 30 2.2.2 Industrial WGR Sample Selection and Preparation ............................................. 31 2.2.3 Cross-link Density Measurements ........................................................................ 32 2.2.4 Atomic Absorption Spectrometry (AAS) ............................................................. 33 2.2.5 Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) ........... 33 2.2.6 CHNS Elemental Analysis ................................................................................... 34 2.2.7 Differential Scanning Calorimetry (DSC) ............................................................ 34 2.2.8 Solid-State 1H NMR Spectroscopy ...................................................................... 34 2.2.9 Thermogravimetric Analysis (TGA) and Thermogravimetry Analysis Coupled with Mass Spectrometry (TGA-MS) ............................................................................. 35 2.3 Results and Discussion ................................................................................................ 35 2.3.1 Preliminary Analysis of WGR by ICP-OES, AAS and CHNS Analysis ............. 35 2.3.2 Solid-state 1H NMR Spectroscopy ....................................................................... 38 2.3.3 Thermogravimetric Analysis (TGA) .................................................................... 40 2.3.4 Thermal Analysis by Differential Scanning Calorimetry ..................................... 50 2.4 Conclusions ................................................................................................................
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