The search for a low cost and effective technique to control and remove volatile organic chemicals (VOCs) has gathered a great attention from the adsorption process field. Advances in manufacturing technology have enabled the creation of activated carbon monoliths (ACM) as promising substitute for traditional packed beds of granular adsorbent materials. The research described in this thesis comprises an extensive experimental study of a single component adsorption process onto square and hexagonal channel Novacarb™ ACM supplied by MAST Carbon Technology Ltd. ACM characterisation methods such as nitrogen and solvent adsorption isotherms, electron microscopy, thermo-gravimetric analysis and thermal dynamic characterization have been used. High BET surface area, high total pore volume and high total solvent mass uptakes have been found. ACM were tested by obtaining column breakthrough curves mainly using dichloromethane and acetone as the adsorbates at the bench-scale. The adsorption dynamics of the ACMs studied were also compared with those of extrudates manufactured by the same process as the ACMs. The influence of humidity on the adsorption process has been studied at the bench-scale. Finally, the adsorption system was scaled-up to about 60cm length monoliths in order to study both adsorption and electrical regeneration taking advantage of the particular electrical properties held by the Novacarb™ ACM. It has been found that ACMs are able to adsorb high levels of VOCs, up to 40% by weight of DCM, good behaviour under humidity conditions and low pressure drop. In contrast, kinetics of ACMs have been found to be somewhat inferior to those of equivalent packed beds, although the ACM performance can be improved by reducing the wall thickness. Adsorption of DCM at the pilot-scale has demonstrated that the Novacarb™ ACM could easily be used in a cyclic thermal swing adsorption process with a half cycle time of less than one hour.

Du fait du coût élevé de certains matériaux adsorbants d’intérêt pour le traitement de la micropollution organique, l’étude a porté sur la régénération de matériaux adsorbants de type zéolithes hydrophobes et monolithe de carbone dans le cas de l’adsorption du bisphénol A et du diclofénac comme micropolluants réfractaires. Des procédés d’oxydation avancée impliquant des espèces radicalaires HO• (réaction de Fenton, électro-Fenton) et SO₄• – (activation de persulfate par voie thermique) ont été utilisés pour assurer la régénération des matériaux par désorption et dégradation oxydative des polluants fixés. La production de radicaux HO• au sein de la phase aqueuse circulant au niveau de l’adsorbant n’est pas suffisamment efficace pour sa régénération. Il a donc été envisagé de générer les radicaux au plus près des molécules adsorbées. Au cours de ce travail, une méthode sensible d’analyse par polarographie de H₂O₂ a été développée et validée pour le suivi des expériences avec les procédés mettant en jeu la réaction de Fenton. Pour différentes zéolithes, le catalyseur de la réaction de Fenton à base de fer a été incorporé préalablement dans la zéolithe. Pour le monolithe de carbone, les propriétés de conduction du matériau ont été mises à profit en l’utilisant comme cathode pour l’application du procédé électro-Fenton permettant de produire les radicaux HO• directement au sein du matériau. Cela a conduit à améliorer les performances de la régénération avec toutefois une diminution de son efficacité au cours de cycles successifs adsorption/régénération. / The elimination of organic micropollutants often requires the use of adsorption processes among the water treatments. The aim of our study is to regenerate two expensive materials (hydrophobic zeolites and carbon monoliths) to increase their life expectancy and decrease their investing cost. Two organic contaminants were targeted : diclofenac and bisphenol A, which are refractory pollutants. Advanced oxidation processes involve radical species, HO• (Fenton and electro-Fenton reactions) and SO₄• – (thermal activation of persulfate ion). These oxidants were used to decompose the adsorbed pollutants and thus regenerate the adsorbents. The HO• production, within the core of aqueous phase, did not reach satisfactory regeneration, and a loss of adsorption capacity was observed. Furthermore, during this study, a sensitive polarographic analytical method was developed and validated for the quantification of H₂O₂ in the aqueous phase. This method was used to follow in situ the Fenton reaction. The location of the catalyst in a closer vicinity of the adsorbed species was then optimized and the iron catalyst was impregnated in the host, prior to the adsorption, on different types of hydrophobic zeolites. Concerning carbon monolith, the electro-Fenton process was carried out using the material as the cathode thanks to its electrical conductivity. Consequently, HO• are produced in the porosity of monolith. This latter property enhanced the degradation of adsorbed solutes. The overall performances were increased compared to the homogeneous Fenton process. Nonetheless, a decrease of the adsorption capacities with adsorption-regeneration cycles was observed.