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(Pp)/ Ground Tire Rubber MANUFACTURING OF POLYPROPYLENE (PP)/ GROUND TIRE RUBBER (GTR) THERMOPLASTIC ELASTOMERS USING ULTRASONICALLY AIDED EXTRUSION A Thesis Presented to The Graduate Faculty of The University of Akron In Partial Fulfillment of the Requirements for the Degree Master of Science Jieruo Liu August, 2013 MANUFACTURING OF POLYPROPYLENE (PP)/ GROUND TIRE RUBBER (GTR) THERMOPLASTIC ELASTOMERS USING ULTRASONICALLY AIDED EXTRUSION Jieruo Liu Thesis Approved: Accepted ______________________ _______________________ Advisor Department Chair Dr. Avraam I. Isayev Dr. Robert Weiss _______________________ _______________________ Committee Member Dean of the College Dr. Thein Kyu Dr. Steven Cheng _______________________ ________________________ Committee Member Dean of the Graduate School Dr. Younjin Min Dr. George Newkome ________________________ Date ii ABSTRACT Compounding ground tire rubber (GTR) from whole waste tires with thermoplastic polyolefins, such as polypropylene (PP), is a possible way to manufacture thermoplastic elastomers and also to recycle waste tires to solve a major environmental problem. The present study looks at the effect of PP/GTR mixing ratio, rubber particle size, type of extruder, maleic anhydride grafted polypropylene (PP-g-MA) compatibilizer and ultrasound on the mechanical and rheological properties of PP and PP/GTR blends. PP and GTR were compounded at ratios of 30/70, 50/50 and 70/30. Whole tire GTR particles of 40 and 140 mesh sizes were used. Both the single screw extruder (SSE) and twin screw extruder (TSE) without and with ultrasonic treatment were applied. PP-g-MA compatibilizer was added to PP/GTR 50/50 blends at concentration of 10 wt %. Rheological, tensile and impact properties of uncompatibilized and compatibilized PP/GTR 50/50 blends were compared. The ultlasonic treatment was carried out at a flow rate of 2 lbs/hr and amplitudes of 5, 7.5 and 10 μm. Pressure and ultrasonic power consumption were measured. The Young’s modulus and the elongation at break of the untreated and ultrasonically treated PP is respectively found to be higher and lower in SSE than that in TSE, with the effect on the tensile strength being insignificant. Complex viscosity of the ultrasonically treated PP changes with amplitude in a complex way depending on the type of extruder. An increase or decrease of viscosity with amplitude is observed. Rubber particles of PP/GTR 50/50 blends of both meshes are reduced in iii sizes, with their roughness increasing more in TSE than in SSE. This leads to a higher viscosity of 50/50 blends in TSE. Complex viscosity of blends from both SSE and TSE increases with an addition of GTR particles. The viscosity of PP/GTR blends of various ratios containing 140 mesh is lower than that of 40 mesh blends. This is due to a lower gel fraction of 140 mesh GTR. Blends with the smaller rubber particle size show much higher elongation at break, indicating a better interaction between the PP and GTR. The addition of the compatibilizer improves mechanical properties of blends. In particular, the tensile strength reaches 19 MPa, and the elongation at break increases to 50%. The highest effect of ultrasound is observed for PP/GTR 70/30 blends. Specifically for PP/GTR 70/30 containing 140 mesh rubber from TSE, the viscosity drops significantly at an amplitude of 10 μm, and the Young’s modulus and elongation at break get improved. This indicates that the breakup of molecular chains leads to creation of macroradicals of components, which recombine, causing an increase in tensile properties. iv ACKNOWLEDGEMENTS The author hopes to express gratitude to her advisor, Dr. Avraam I. Isayev, for his patient and kind instructions on research and courses. The author also would like to thank to Dr. Jaesun Choi, Mr. Todd M. Lewis, Mr. Tian Liang and Mr. Keyuan Huang for their great help. v TABLE OF CONTENTS Page LIST OF FIGURES…………………………………………………………………ix CHAPTER I. INTRODUCTION................................................................................. …………..1 II. LITERATURE SURVEY......................................................................................4 2.1. Brief Introdcution of Rubber Recycling..........................................................4 2.2. Plastic/Rubber based Thermoplastic Elastomers..............................................4 2.3. Polyolefin-based thermoplastic elastomers （TPO）.....................................5 2.4. Thermoplastic vulcanizates (TPVs) .................................................................6 2.5 Compatibility between plastic and rubber..........................................................6 2.5.1. Modification of rubber............................................................................7 2.5.1.1. Physical methods………………………………………………7 2.5.1.2. Chemical methods……………………………………..………8 2.5.2. Compatibilizer……………………………………………………..….11 vi 2.6 Ultrasound…………………………………………………………………..12 2.6.1. Effect of ultrasound on polymers………………………………….…..14 2.6.1.1. Degradation of polymer by ultrasound……………………….14 2.6.1.2. Devulcaniation of rubber by ultrasound………………...…….15 2.6.1.3. Compatibilization of blends by ultrasound……………………17 2.6.1.4 Application of ultrasound in filled polymer system….……….19 III EXPERIMENTAL..................................................................................................21 3.1. Materials .........................................................................................................21 3.2 Extruders with ultrasound treatment...............................................................22 3.2.1. Preparation of blends in single screw extruder……………….….……24 3.2.2. Preparation of blends in twin screw extruder…………………….…….25 3.3. Molding...........................................................................................................26 3.3.1. Injection molding ..................................................................................26 3.3.2. Compression molding ..........................................................................26 3.4 Characterization................................................................................................26 3.4.1. Rheological measurements……………………….……………………26 3.4.2. Tensile tests............................................................................................27 vii 3.4.3. Impact tests.............................................................................................27 3.4.4. Morphological measurements................................................................28 IV RESULTS AND DISCUSSION.............................................................................29 4.1. Die pressure.....................................................................................................29 4.2. Power consumption of ultrasound……..........................................................31 4.3. Rheology........................................................................................................34 4.4. Tensile properties...........................................................................................44 4.5 Impact test……………………………………………………………………57 4.6 Morphological test…………..........................................................................59 V SUMMARY.............................................................................................................62 REFERENCES.............................................................................................................64 viii LIST OF FIGURES Figure Page 2.1 Ultrasound cavitation bubble growth and collapse ….....................................……………………………...14 2.2 Schematic of the overstressed network fragment around the collapsing bubble…………………………...16 3.1 Schematic drawing of single screw extruder…………………………………..22 3.2 Design of 33:1 screw with two mixing sections before the ultrasonic treatment section and a conveying screw flights after it….........23 3.3 Schematic drawing of twin screw extruder……………………………………24 4.1 Die pressure of 40 mesh blends from SSE (a) and 140 mesh blends from SSE (b)………………………..………………..…30 4.2 Power consumption of 40 mesh blends from SSE (a), TSE (b), 140 mesh blends from SSE (c) and TSE (d)…………………………………….33 4.3 Complex viscosity of 40 mesh blends from SSE………………………………35 4.4 Complex viscosity of 140 mesh blends from SSE……………………………..38 4.5 Complex viscosity of 40 mesh blends from TSE……………………………….39 4.6 Complex viscosity of 140 mesh blends from TSE………………………………41 4.7 Complex viscosity for PP/GTR/PP-g-MA 50/50/10 and 50/50/0, 40 mesh blends from SSE (a), TSE (b), 140 mesh blends from SSE (c) and TSE (d) ………….42 4.8 Cole-Cole plot for PP/GTR/PP-g-MA 50/50/10 and 50/50/0, 40 mesh blends from SSE (a), TSE (b), 140 mesh blends from SSE (c) and TSE (d) …………..43 4.9 Young’s modulus (a), tensile strength (b) and elongation at break (c) for pure PP from both SSE and TSE as a function of ultrasonic amplitude…………………45 4.10 Young’s modulus (a), tensile strength (b) and elongation at break (c) of 40 mesh blends from SSE against ultrasonic amplitude ……………………………….46 ix 4.11 Young’s modulus (a), tensile strength (b) and elongation at break (c) of 40 mesh blends from SSE against PP weight percentage………………..……………47 4.12 Young’s modulus (a), tensile strength (b) and elongation at break (c) of 140 mesh blends from SSE against ultrasonic amplitude………………………….49 4.13 Young’s modulus (a), tensile strength (b) and elongation at break (c) of 140 mesh blends from SSE against PP weight percentage……………..….………50 4.14 Young’s modulus (a), tensile strength (b) and elongation
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