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The waste rubber and end-of-life tires management has become a serious environmental problem. It is well known that the best way to carry out the disposal of these wastes is through recycling by devulcanization. Therefore, in the last decades, many methods have been developed to perform this treatment. Nevertheless, the degree and quality of the achieved devulcanization is still difficult to evaluate. The Horikx theory is an approach often used for this purpose. Hence, in this work, the validity of this theory was experimentally checked. The theoretical curve that represents crosslink scission was experimentally built for sulfur-cured natural rubber, sulfur-cured natural rubber reinforced with carbon black, sulfur-cured ethylene propylene diene monomer rubber and peroxide-cured ethylene propylene diene monomer rubber. Several samples with vulcanization (or devulcanization) degree ranging from 0 to 100% were processed, and the corresponding soluble fractions and crosslink densities were measured by the swelling test. The experimental results were in good agreement with the theoretical predictions, independently of the studied material, fact that confirms the validity of the Horikx approach. This finding will contribute to improve the waste rubber devulcanization, and therefore to progress in the environmental protection.

This work is focused on the recycling of natural rubber industry waste by means of thermo-mechanical devulcanization. With that aim, tests were carried out in an industrial twin-screw extruder, at different barrel temperatures, ranging from 80 to 220 °C. The extrusion was done with a screw profile specifically designed for the devulcanization process. The extent and quality of devulcanization were evaluated through the measurements of crosslink density, soluble fraction and Mooney viscosity, and by using the Horikx diagram. Results showed that a high degree of reclaiming (˜90%) was obtained, independently of the barrel temperature. The samples with the best devulcanization quality, i.e. the samples with a more selective sulfur bond scission, were found to be those treated at a lower input temperature. This was explained by the effect of the rubber homogenous self-heating which contributes to the local increase of the material temperature, during the devulcanization process. Moreover, it was found that the properties of the devulcanized rubber/virgin rubber blends were not significantly affected by the addition of the treated rubber. Results suggest that the entire natural rubber industry waste could be recycled into new competitive products, with low energy consumption. This would present a real contribution to the industrial recycling and thus a noticeable improvement of the environment.

The elimination of rubber wastes without affecting the environment is one of the most important challenges of the 21st century waste management. Accordingly, the present work is focused on the recycling of natural rubber (NR) industry waste by means of devulcanization in supercritical carbon dioxide (scCO2) atmosphere. With that aim, a novel device allowing to perform rubber devulcanization was developed. It consists of a triaxial compression reactor integrated into a dynamic hydraulic universal testing machine with a heating chamber. NR industry waste was devulcanized in the mentioned device at different temperatures, in scCO2 by using diphenyl disulfide (DD) as devulcanizing reagent. The devulcanization degree and quality of the treated materials were evaluated by the swelling test combined with the Horikx theory. It was appeared that a successful devulcanization, with almost no degradation, was obtained, and the devulcanization degree reached maximum value of ~90%. Thermogravimetric tests and scanning electron microscopy (SEM) images strengthened these results. Finally, it was concluded that the developed device is appropriate to perform rubber recycling, which contributes to the progress in the environmental protection.

This study focused on the possibility of recycling Waste Tire Rubber (WTR) to be used as polymer modifier. Thus, WTR was grinded into powder, at ambient temperature, with a disc mill PQ500 and microwave electromagnetic energy was used to devulcanize this powder with the final aim of producing a new composite by its incorporation in a thermoset resin. The influence of the treatment microwave energy on the devulcanization ratio was investigated. FTIR analysis revealed that rupture of Sulfur-Sulfur (SAS) and Carbon-Sulfur (CAS) bonds have occurred during the treatment. Swelling analysis showed that the microwave treatment can lead to a very significant degree of devulcanization. The Ground Tire Rubber (GTR) and the Devulcanized Ground Tire Rubber (DGTR) were then separately used to prepare epoxy based composites. It appeared that epoxy composites filled with DGTR have better mechanical properties than those filled with untreated GTR. This result agrees with scanning electron microscopy observations which highlighted a better interface coherence between DGTR and epoxy. A complementary analysis pointed out a linear relationship between the rubber modulus and the number of crosslink per chain. Fil: Aoudia, Karima. Universite Mouloud Mammeri de Tizi-ouzou; Argelia Fil: Azem, Saïd. Universite Mouloud Mammeri de Tizi-ouzou; Argelia Fil: Aït Hocine, Nourredine. Institut National des Sciences Appliquées; Francia Fil: Gratton, Michel. Institut National des Sciences Appliquées ; Francia Fil: Pettarin, Valeria. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina Fil: Seghar, Saïd. Phenix Technolgies; Francia

Disposal of used tires and rubber wastes is one of the biggest challenges of the 21st century waste management. One of the environmentally friendly possibilities of recycling this type of material is to go through the breaking of their three-dimensional structure. This treatment, called the devulcanization, can be defined as a process that causes the selective breakup of the sulfur-sulfur (S-S) and carbon-sulfur (C-S) chemical bonds without breaking the backbone network and without degrading the material. The devulcanized rubber can be mixed with virgin rubber or with other kinds of matrices to give new compounds without generating a significant decrease in mechanical and physical properties. Many devulcanization process types are presented in the literature: chemical, ultrasound, microwave, thermomechanical, etc. The thermomechanical devulcanization based on extrusion seems to be the more suitable to be applied on an industrial scale. The supercritical CO2 has been proposed as a green atmosphere that can be used to improve this type of devulcanization. In fact, it seems that in supercritical conditions, the CO2 swells the rubber and stretches the sulfide links, making them easier to break. This paper presents a literature review on rubbers recycling by devulcanization. It is focused on the different devulcanization techniques used in the last decades. Particular attention is paid to the thermomechanical method, those in the presence of supercritical CO2 and, finally, the combined thermomechanical process with supercritical CO2 atmosphere.

International audience; In this study, styrene butadiene rubber (SBR) was devulcanized using microwave irradiation. In particular, effectof ionic liquid (IL), pyrrolidinium hydrogen sulfate [Pyrr][HSO4], on the devulcanization performance was studied. It wasobserved that the evolution of the temperature reached by rubber powder exposed to microwave irradiation for differentenergy values was favored by the presence of ionic liquid [Pyrr][HSO4] significantly over the whole range of themicrowave energy values. Beyond the threshold point of 220 Wh/kg, the soluble fraction after devulcanization sharplyincreased with increasing devulcanization microwave energy. For the powder mixed with [Pyrr][HSO4], the increase wasmore significant. Furthermore, the crosslink density was observed to decrease slowly with the microwave energy up to220 Wh/kg, beyond which the crosslink density decreased significantly for the rubber impregnated with IL. For the rubberwith IL, significant and continuous increase in Tg with microwave energy values was observed in comparison with the SBRwhere no change in transition temperature was observed. Mechanical shearing of rubber gums in the two-roll mill favoredthe devulcanization process, which indicated that the combination of mechanical loading with microwave energy and IL isan efficient procedure allowing an optimal devulcanization of rubbers.