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Keywords = Horikx

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21 pages, 5683 KiB  
Article
Recycling of EPDM via Continuous Thermo-Mechanical Devulcanization with Co-Rotating Twin-Screw Extruder
by Valentina Brunella, Veronica Aresti, Umberto Romagnolli, Bruno Muscato, Marco Girotto, Paola Rizzi and Maria Paola Luda
Polymers 2022, 14(22), 4853; https://doi.org/10.3390/polym14224853 - 11 Nov 2022
Cited by 11 | Viewed by 4741
Abstract
Devulcanization represents the recycling of choice for a homogenous rubber waste stream because it allows revulcanization of samples previously devulcanized, making the life of the rubber virtually endless, according to the principles of circular economy. Among the many devulcanization processes, the thermo-mechanical one [...] Read more.
Devulcanization represents the recycling of choice for a homogenous rubber waste stream because it allows revulcanization of samples previously devulcanized, making the life of the rubber virtually endless, according to the principles of circular economy. Among the many devulcanization processes, the thermo-mechanical one is the most appealing because it is a continuous process, easy to be industrialized. In this paper a comprehensive set of analyses (FTIR, TGA, DSC, elemental analyses, Py-GC/MS, swelling tests) were carried out on a post-industrial ethylene propylene diene monomer (EPDM), thermo-mechanical devulcanized in a co-rotating twin-screw extruder with different process parameters (thermal and screw profile, rpm). Results of the swelling test according to the Flory–Rehner theory and Horikx analyses show that the higher the thermal profile and the higher the rpm, the higher is the percentage of devulcanization. The quality of the devulcanized sample in terms of sol fraction and percentage of random scissions depends on the process conditions. The screw profile concurs to the efficiency of the devulcanization: the different number of kneading elements and more in general the screw profile composition affects the percentage of devulcanization, making the results in some tests more dependent on the screw speed. Full article
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19 pages, 3151 KiB  
Article
Setting Relationships between Structure and Devulcanization of Ground Tire Rubber and Their Effect on Self-Healing Elastomers
by Luis E. Alonso Pastor, Karina C. Núñez Carrero, Javier Araujo-Morera, Marianella Hernández Santana and José María Pastor
Polymers 2022, 14(1), 11; https://doi.org/10.3390/polym14010011 - 21 Dec 2021
Cited by 12 | Viewed by 5162
Abstract
The use of devulcanized tire powder as an effective reinforcement in self-healing styrene-butadiene rubber (SBR) compounds has been investigated for the first time in this work. For this purpose, the evolution of the microstructure of the rubber from end-of-life tires (ELTs) was studied [...] Read more.
The use of devulcanized tire powder as an effective reinforcement in self-healing styrene-butadiene rubber (SBR) compounds has been investigated for the first time in this work. For this purpose, the evolution of the microstructure of the rubber from end-of-life tires (ELTs) was studied during granulation, grinding and devulcanization through an exhaustive characterization work in order to relate the final microstructure with the mechanical response of the repaired systems. Different morphologies (particle size distribution and specific surface area) obtained by cryogenic and water jet grinding processes, as well as different devulcanization techniques (thermo-mechanical, microwave, and thermo-chemical), were analyzed. The results demonstrated the key influence of the morphology of the ground tire rubber (GTR) on the obtained devulcanized products (dGTR). The predictions of the Horikx curves regarding the selectivity of the applied devulcanization processes were validated, thereby; a model of the microstructure of these materials was defined. This model made it possible to relate the morphology of GTR and dGTR with their activity as reinforcement in self-healing formulations. In this sense, higher specific surface area and percentage of free surface polymeric chains resulted in better mechanical performance and more effective healing. Such a strategy enabled an overall healing efficiency of more than 80% in terms of a real mechanical recovery (tensile strength and elongation at break), when adding 30 phr of dGTR. These results open a great opportunity to find the desired balance between the mechanical properties before and after self-repair, thus providing a high technological valorization to waste tires. Full article
(This article belongs to the Special Issue Advances in Rubber Elastomer)
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25 pages, 7078 KiB  
Article
Best Practice for De-Vulcanization of Waste Passenger Car Tire Rubber Granulate Using 2-2-dibenzamidodiphenyldisulfide as De-Vulcanization Agent in a Twin-Screw Extruder
by Hans van Hoek, Jacques Noordermeer, Geert Heideman, Anke Blume and Wilma Dierkes
Polymers 2021, 13(7), 1139; https://doi.org/10.3390/polym13071139 - 2 Apr 2021
Cited by 11 | Viewed by 3709
Abstract
De-vulcanization of rubber has been shown to be a viable process to reuse this valuable material. The purpose of the de-vulcanization is to release the crosslinked nature of the highly elastic tire rubber granulate. For present day passenger car tires containing the synthetic [...] Read more.
De-vulcanization of rubber has been shown to be a viable process to reuse this valuable material. The purpose of the de-vulcanization is to release the crosslinked nature of the highly elastic tire rubber granulate. For present day passenger car tires containing the synthetic rubbers Styrene-Butadiene Rubber (SBR) and Butadiene Rubber (BR) and a high amount of silica as reinforcing filler, producing high quality devulcanizate is a major challenge. In previous research a thermo-chemical mechanical approach was developed, using a twin-screw extruder and diphenyldisulfide (DPDS) as de-vulcanization agent.The screw configuration was designed for low shear in order to protect the polymers from chain scission, or uncontrolled spontaneuous recombination which is the largest problem involved in de-vulcanization of passenger car tire rubber. Because of disadvantages of DPDS for commercial use, 2-2-dibenzamidodiphenyldisulfide (DBD) was used in the present study. Due to its high melting point of 140 °C the twin-screw extruder process needed to be redesigned. Subsequent milling of the devulcanizate at 60 °C with a narrow gap-width between the mill rolls greatly improved the quality of the devulcanizate in terms of coherence and tensile properties after renewed vulcanization. As the composition of passenger car tire granulate is very complex, the usefulness of the Horikx-Verbruggen analysis as optimization parameter for the de-vulcanization process was limited. Instead, stress-strain properties of re-vulcanized de-vulcanizates were used. The capacity of the twin-screw extruder was limited by the required residence time, implying a low screw speed. A best tensile strength of 8 MPa at a strain at break of 160% of the unblended renewed vulcanizate was found under optimal conditions. Full article
(This article belongs to the Section Circular and Green Sustainable Polymer Science)
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15 pages, 3471 KiB  
Article
Thermomechanical Devulcanisation of Ethylene Propylene Diene Monomer (EPDM) Rubber and Its Subsequent Reintegration into Virgin Rubber
by Dávid Zoltán Pirityi and Kornél Pölöskei
Polymers 2021, 13(7), 1116; https://doi.org/10.3390/polym13071116 - 1 Apr 2021
Cited by 24 | Viewed by 5693
Abstract
Rubber waste remains a challenge for material science because its covalently cross-linked structure hinders the establishment of the circular economy of rubber. Devulcanisation may provide a solution, as it converts rubber vulcanisates back into their original, uncured state. Devulcanised rubber may be revulcanised [...] Read more.
Rubber waste remains a challenge for material science because its covalently cross-linked structure hinders the establishment of the circular economy of rubber. Devulcanisation may provide a solution, as it converts rubber vulcanisates back into their original, uncured state. Devulcanised rubber may be revulcanised or incorporated into virgin rubber, thus waste is utilized and the use of primary resources is reduced at the same time. In this paper, we treated sulphur-cured EPDM (ethylene propylene diene monomer) rubber on a two-roll mill at various temperatures and frictions. We determined the effectiveness of devulcanisation via Horikx’s analysis, which suggested that low devulcanisation temperatures would result in a 50% decrease in cross-link density with minimal polymer degradation. The devulcanisate was recycled via two methods: (a) revulcanisation with extra curing agents, and (b) mixing it with various amounts of the original rubber mixture, preparing rubber samples with 25, 50, 75, and 100 wt% recycled content. Tensile tests revealed that the samples’ elastic properties were severely compromised at 75 and 100 wt% devulcanisate contents. However, tensile strength decreased only by 15% and 20% for revulcanisates containing 25% and 50% recycled rubber, respectively. Full article
(This article belongs to the Special Issue Chemical Recycling of Polymers)
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17 pages, 2284 KiB  
Article
Upscaling of a Batch De-Vulcanization Process for Ground Car Tire Rubber to a Continuous Process in a Twin Screw Extruder
by Sitisaiyidah Saiwari, Johannes W. Van Hoek, Wilma K. Dierkes, Louis E.A.M. Reuvekamp, Geert Heideman, Anke Blume and Jacques W.M. Noordermeer
Materials 2016, 9(9), 724; https://doi.org/10.3390/ma9090724 - 24 Aug 2016
Cited by 29 | Viewed by 6519
Abstract
As a means to decrease the amount of waste tires and to re-use tire rubber for new tires, devulcanization of ground passenger car tires is a promising process. Being an established process for NR and EPDM, earlier work has shown that for ground [...] Read more.
As a means to decrease the amount of waste tires and to re-use tire rubber for new tires, devulcanization of ground passenger car tires is a promising process. Being an established process for NR and EPDM, earlier work has shown that for ground passenger car tire rubber with a relatively high amount of SBR, a devulcanization process can be formulated, as well. This was proven for a laboratory-scale batch process in an internal mixer, using diphenyl disulfide as the devulcanization aid and powder-sized material. In this paper, the devulcanization process for passenger car tire rubber is upscaled from 15 g per batch and transformed into a continuous process in a co-rotating twin screw extruder with a capacity of 2 kg/h. As SBR is rather sensitive to devulcanization process conditions, such as thermal and mechanical energy input, the screw design was based on a low shear concept. A granulate with particle sizes from 1–3.5 mm was chosen for purity, as well as economic reasons. The devulcanization process conditions were fine-tuned in terms of: devulcanization conditions (time/temperature profile, concentration of devulcanization aid), extruder parameters (screw configuration, screw speed, fill factor) and ancillary equipment (pre-treatment, extrudate handling). The influence of these parameters on the devulcanization efficiency and the quality of the final product will be discussed. The ratio of random to crosslink scission as determined by a Horikx plot was taken for the evaluation of the process and material. A best practice for continuous devulcanization will be given. Full article
(This article belongs to the Special Issue Advances in Research on Elastomers)
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