Souad Rakass

Synthesis, characterization and photocatalytic activity of α-Bi2O3 nanoparticles

Abstract Monoclinic bismuth oxide α-Bi2O3 nanoparticles were synthesized starting from a mixture of oxalate complexes of bismuth Bi(C2O4)OH and Bi2(C2O4)3·xH2O obtained by a direct solid-state reaction between a nitrate salt of bismuth and oxalic acid. The starting oxalate mixture precursors were studied by thermal gravimetric analysis (TGA) and characterized by Fourier transform infrared spectroscopy (FTIR). After heat treatment of the oxalate precursors, the obtained oxide α-Bi2O3 was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). These α-Bi2O3 nanoparticles show low efficiency in photodegradation under UV light irradiation of the dye rhodamine B.

Preparation and Characterization of α-Zinc Molybdate Catalyst: Efficient Sorbent for Methylene Blue and Reduction of 3-Nitrophenol

Zinc molybdate (ZnMoO4) was prepared by thermal decomposition of an oxalate complex under a controlled temperature of 500 °C. Analyses of the oxalate complex were carried out using Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). On the other hand, analyses of the synthesized zinc molybdate were carried out by X-ray diffraction (XRD), transmission electron microscopy (TEM), and Brunauer-Emmett-Teller technique (BET). The efficiency of the synthesized catalyst was tested with the reduction reaction of 3-nitrophenol (3-NP), and was also applied as a sorbent for methylene blue dye (MB) in aqueous solutions. The catalytic test of zinc molybdate shows a very high activity. The concentration reduction progress and adsorption of the dye were followed by an ultraviolet-visible (UV-vis) spectrophotometer.

Modified Nigella Sativa Seeds as a Novel Efficient Natural Adsorbent for Removal of Methylene Blue Dye

The aim of this work was to investigate the use of modified nigella sativa seeds (MNS) for removing of methylene blue (MB) dye from aqueous solution. The nigella sativa (NS) seeds have been pre-treated at different temperatures and periods of time. The maximum adsorption of MB was achieved using NS sample washed with distilled water pre-heated at 65 °C for one hour, then ground to 250 µm particle size (MNS-4). Different parameters were modified to optimize the removal process of MB using MNS-4, such as contact times, temperatures, initial dye concentrations, adsorbent doses, and pH of the solution. MNS-4 exhibited a removal efficiency of 99% for initial dye concentrations greater than 800 ppm at pH value of 11. The kinetic study indicated that the removal process follows the pseudo second order model. The removal was spontaneous, endothermic and favorable, and this was indicated by the thermodynamic study. Maximum removal capacity was 194 mg/g as deduced from Langmuir model. The removal efficiency was maintained after four recycle uses. The modified nigella sativa seeds were characterized before, and after adsorption and regeneration by Fourier Transform infrared (FTIR) and scanning electron microscopy (SEM). The data suggested that nigella sativa seeds could be a prospective agent for removing MB from wastewater.

High Catalytic Efficiency of Nanostructured β-CoMoO4 in the Reduction of the Ortho-, Meta- and Para-Nitrophenol Isomers

Nanostructured β-CoMoO4 catalysts have been prepared via the thermal decomposition of an oxalate precursor. The catalyst was characterized by infrared spectroscopy (FTIR), X-ray diffraction (XRD), Brunauer-Emmett-Teller method (BET), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM). The efficiency of these nanoparticles in the reduction of ortho- and meta-nitrophenol isomers (2-NP, 3-NP, and 4-NP) to their corresponding aminophenols was tested using UV-visible spectroscopy measurements. It was found that, with a β-CoMoO4 catalyst, NaBH4 reduces 3-NP instantaneously, whilst the reduction of 2-NP and 4-NP is slower at 8 min. This difference is thought to arise from the lower acidity of 3-NP, where the negative charge of the phenolate could not be delocalized onto the oxygen atoms of the meta-nitro group.

Enhanced catalytic reduction of para-nitrophenol using α-MoO3 molybdenum oxide nanorods and stacked nanoplates as catalysts prepared from different precursors

ABSTRACT Molybdenum oxide, α-MoO3, nanorods and stacked nanoplates were prepared from oxalate, citrate and tartrate precursors. These molybdenum oxides showed high efficiencies in the reduction of para-nitrophenol to para-aminophenol in the presence of NaBH4. The prepared precursors were first characterized by thermal gravimetric analysis (TGA) and then thermally decomposed at 350°C (oxalate precursor) and 550°C (citrate and tartrate precursors). The final oxides were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and the Braunauer–Emmet–Teller (BET) technique. The oxalate precursor is the most efficient catalyst for the reduction reaction.

Application of Organo-Magadiites for the Removal of Eosin Dye from Aqueous Solutions: Thermal Treatment and Regeneration

Na-magadiite exchanged with cetyl-trimethylammonium cations provided organophilic silicate materials that allowed for the effective removal of the acidic dye “eosin”. The organic cations were intercalated into the interlayer spacing of the layered silicate via an exchange reaction between the organic cations from their bromide salt and the solid Na-magadiite at room temperature. Different techniques were used to characterize the effect of the initial concentration of the surfactant on the structure of the organo-magadiites. The C, H, and N analysis indicated that a maximum of organic cations of 0.97 mmol/g was achieved and was accompanied by an expansion of the basal spacing of 3.08 nm, with a tilted angle of 59° to the silicate layers. The conformation of the organic surfactants was probed using solid-state 13C, finding mainly the trans conformation similar to that of the starting cetyl trimethylammonium bromide salt (C16TMABr). Thermal gravimetric analysis was carried out to study the thermal stability of the resulting organo-magadiites. The intercalated surfactants started to decompose at 200 °C, with a mass loss percentage of 8% to 25%, depending on the initial loading of the surfactant, and was accompanied by a decrease of the basal spacing from 3.16 nm to 2.51 nm, as deduced from the in situ X-ray diffraction studies. At temperatures below 220 °C, an expansion of the basal spacing from 3.15 to 3.34 nm occurred. These materials were used as a removal agent for the anionic dye eosin. The maximum amount of the dye removed was related to the organic cation content and to the initial concentration of eosin, with an improvement from 2.5 mg/g to 80.65 mg/g. This value decreased when the organo-magadiite was preheated at temperatures above 200 °C. The regeneration tests indicated that an 85% removal efficiency was maintained after six cycles of use for the organo-magadiite using Ci of 200 mg/L.

Removal Properties of Anionic Dye Eosin by Cetyltrimethylammonium Organo-Clays: The Effect of Counter-Ions and Regeneration Studies

The organo-clays (OCs) were prepared by a cation exchange reaction between surfactant (cetyltrimethylammonium, C16TMA) from different counterions (Bromide, Chloride, and Hydroxide). The effect of the counterions was investigated on the physico-chemical properties of the prepared organo-clays. The highest uptake of organic cations (1.60 mmol/g) was achieved using cetyl trimethylammonium bromide solution and the lowest value (0.93 mmol/g) was obtained after modification with cetyl trimethylammonium hydroxide solution starting from the same initial ratio of mmol/g of clay greater than 2.40. The arrangement of C16TMA cations within the interlayer space was assumed to be perpendicular with a tilt angle of 32° to the plane of clay sheets instead of being parallel to the clay surface using C16TMAOH solution at the same ratio. Different techniques were used to characterize these materials. The thermal stability of these organ-clays was investigated using an in-situ X-ray diffraction (XRD) technique. The decomposition of the surfactant moiety occurred at temperatures higher than 215 °C and was accompanied with a shrinkage of the basal spacing value to 1.42 nm. These materials were applied in the removal of an acid dye “eosin.” The removed amount of eosin depended on the initial concentrations and the content of surfactants in the organo-clays. The removal of eosin was found to be an endothermic process. The maximum amount of 90 mg/g was achieved. The preheated treatment temperature of two selected OCs did affect the removal properties of eosin. A progressive reduction was observed at temperatures higher than 200 °C. The regeneration of spent OCs was studied and acceptable removal efficiency was maintained after 4 to 6 cycles depending on the used initial concentrations.

Molybdenum Trioxide: Efficient Nanosorbent for Removal of Methylene Blue Dye from Aqueous Solutions

Nano Molybdenum trioxide (α-MoO3) was synthesized in an easy and efficient approach. The removal of methylene blue (MB) in aqueous solutions was studied using this material. The effects of various experimental parameters, for example contact time, pH, temperature and initial MB concentration on removal capacity were explored. The removal of MB was significantly affected by pH and temperature and higher values resulted in increase of removal capacity of MB. The removal efficiency of Methylene blue was 100% at pH = 11 for initial dye concentrations lower than 150 ppm, with a maximum removal capacity of 152 mg/g of MB as gathered from Langmuir model. By comparing the kinetic models (pseudo first-order, pseudo second-order and intraparticle diffusion model) at various conditions, it has been found that the pseudo second-order kinetic model correlates with the experimental data well. The thermodynamic study indicated that the removal was endothermic, spontaneous and favorable. The thermal regeneration studies indicated that the removal efficiency (99%) was maintained after four cycles of use. Fourier Transform Infrared (FTIR) and Scanning Electron Microscopy (SEM) confirmed the presence of the MB dye on the α-MoO3 nanoparticles after adsorption and regeneration. The α-MoO3 nanosorbent showed excellent removal efficiency before and after regeneration, suggesting that it can be used as a promising adsorbent for removing Methylene blue dye from wastewater.