Search results for: immobilized TiO₂

Authors: J. Tirano, H. Zea, C. Luhrs

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Photocatalysis has established as viable option in the development of processes for the treatment of pollutants and clean energy production. This option is based on the ability of semiconductors to generate an electron flow by means of the interaction with solar radiation. Owing to its electronic structure, TiO₂ is the most frequently used semiconductors in photocatalysis, although it has a high recombination of photogenerated charges and low solar energy absorption. An alternative to reduce these limitations is the use of nanostructured morphologies which can be produced during the synthesis of TiO₂ nanotubes (TNTs). Therefore, if possible to produce vertically oriented nanostructures it will be possible to generate a greater contact area with electrolyte and better charge transfer. At present, however, the development of these innovative structures still presents an important challenge for the development of competitive photoelectrochemical devices. This research focuses on established correlations between synthesis variables and 1D nanostructure morphology which has a direct effect on the photocatalytic performance. TNTs with controlled morphology were synthesized by two-step potentiostatic anodization of titanium foil. The anodization was carried out at room temperature in an electrolyte composed of ammonium fluoride, deionized water and ethylene glycol. Consequent thermal annealing of as-prepared TNTs was conducted in the air between 450 °C-550 °C. Morphology and crystalline phase of the TNTs were carried out by SEM, EDS and XRD analysis. As results, the synthesis conditions were established to produce nanostructures with specific morphological characteristics. Anatase was the predominant phase of TNTs after thermal treatment. Nanotubes with 10 μm in length, 40 nm in pore diameter and a surface-volume ratio of 50 are important in photoelectrochemical applications based on TiO₂ due to their 1D characteristics, high surface-volume ratio, reduced radial dimensions and high oxide/electrolyte interface. Finally, this knowledge can be used to improve the photocatalytic activity of TNTs by making additional surface modifications with dopants that improve their efficiency.

Keywords: electrochemical anodization, morphology, self-organized nanotubes, TiO₂ nanotubes

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Authors: A. Apostolopoulou, D. Sygkridou, A. N. Kalarakis, E. Stathatos

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Mesoscopic perovskite solar cells (mp-PSCs) with mesoporous bilayer were fabricated under ambient conditions. The bilayer was formed by capping the mesoporous TiO₂ layer with a layer of In₂O₃. CH₃NH₃I_3-xCl_x mixed halide perovskite was prepared through the one-step method and was used as the light absorber. The mp-PSCs with the composite TiO₂/In₂O₃ mesoporous layer exhibited optimized electrical parameters, compared with the PSCs that employed only a TiO₂ mesoporous layer, with a current density of 23.86 mA/cm², open circuit voltage of 0.863 V, fill factor of 0.6 and a power conversion efficiency of 11.2%. These results indicate that the formation of a proper semiconductor capping layer over the basic TiO₂ mesoporous layer can facilitate the electron transfer, suppress the recombination and subsequently lead to higher charge collection efficiency.

Keywords: ambient conditions, high efficiency solar cells, mesoscopic perovskite solar cells, TiO₂ / In₂O₃ bilayer

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Authors: Priya Ruban, Thirunavoukkarasu Manikkannan, Sakthivel Ramasamy

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Sulfide is one of the major pollutants of tannery effluent which is mainly generated during the process of unhairing. Recovery of Hydrogen green fuel from sulfide wastewater using photocatalysis is a ‘Cleaner Production Method’, since renewable solar energy is utilized. It has triple advantages of the generation of H2, waste minimization and odor or pollution control. Designing of safe and green photocatalysts and developing suitable solar photoreactor is important for promoting this technology to large-scale application. In this study, green photocatalyst i.e., spinach derived carbon dots (SCDs 5 wt % and 10 wt %)/TiO2 nanocomposite was synthesized for generation of H2 from sulfide wastewater using lab-scale solar photocatalytic reactor. The physical characterization of the synthesized solar light responsive nanocomposites were studied by using DRS UV-Vis, XRD, FTIR and FESEM analysis. The absorption edge of TiO2 nanoparticles is extended to visible region by the incorporation of SCDs, which was used for converting noxious pollutant sulfide into eco-friendly solar fuel H2. The SCDs (10 wt%)-TiO2 nanocomposite exhibits enhanced photocatalytic hydrogen production i.e. ~27 mL of H2 (180 min) from simulated sulfide wastewater under LED visible light irradiation which is higher as compared to SCDs. The enhancement in the photocatalytic generation of H2 is attributed to combining of SCDs which increased the charge mobility. This work may provide new insights to usage of naturally available and cheap materials to design novel nanocomposite as a visible light active photocatalyst for the generation of H2 from sulfide containing wastewater.

Keywords: carbon dots, hydrogen fuel, hydrogen sulfide, photocatalysis, sulfide wastewater

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Authors: Mayoorika Shukla, Pramila Jakhar, Tejendra Dixit, I. A. Palani, Vipul Singh

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Biosensors are analytical devices with wide range of applications in biological, chemical, environmental and clinical analysis. It comprises of bio-recognition layer which has biomolecules (enzymes, antibodies, DNA, etc.) immobilized over it for detection of analyte and transducer which converts the biological signal into the electrical signal. The performance of biosensor primarily the depends on the bio-recognition layer and therefore it has to be chosen wisely. In this regard, nanostructures of metal oxides such as ZnO, SnO2, V2O5, and TiO2, etc. have been explored extensively as bio-recognition layer. Recently, ZnO has the attracted attention of researchers due to its unique properties like high iso-electric point, biocompatibility, stability, high electron mobility and high electron binding energy, etc. Although there have been many reports on usage of ZnO as bio-recognition layer but to the authors’ knowledge, none has ever observed correlation between optical properties like defect suppression and biosensing capability of the sensor. Here, ZnO nanorods (ZNR) have been synthesized by a low cost, simple and low-temperature hydrothermal growth process, over Platinum (Pt) coated glass substrate. The ZNR have been synthesized in two steps viz. initially a seed layer was coated over substrate (Pt coated glass) followed by immersion of it into nutrient solution of Zinc nitrate and Hexamethylenetetramine (HMTA) with in situ addition of KMnO4. The addition of KMnO4 was observed to have a profound effect over the growth rate anisotropy of ZnO nanostructures. Clustered and powdery growth of ZnO was observed without addition of KMnO4, although by addition of it during the growth, uniform and crystalline ZNR were found to be grown over the substrate. Moreover, the same has resulted in suppression of defects as observed by Normalized Photoluminescence (PL) spectra since KMnO4 is a strong oxidizing agent which provides an oxygen rich growth environment. Further, to explore the correlation between defect suppression and biosensing capability of the ZNR Glucose oxidase (Gox) was immobilized over it, using physical adsorption technique followed by drop casting of nafion. Here the main objective of the work was to analyze effect of defect suppression over biosensing capability, and therefore Gox has been chosen as model enzyme, and electrochemical amperometric glucose detection was performed. The incorporation of KMnO4 during growth has resulted in variation of optical and charge transfer properties of ZNR which in turn were observed to have deep impact on biosensor figure of merits. The sensitivity of biosensor was found to increase by 12-18 times, due to variations introduced by addition of KMnO4 during growth. The amperometric detection of glucose in continuously stirred buffer solution was performed. Interestingly, defect suppression has been observed to contribute towards the improvement of biosensor performance. The detailed mechanism of growth of ZNR along with the overall influence of defect suppression on the sensing capabilities of the resulting enzymatic electrochemical biosensor and different figure of merits of the biosensor (Glass/Pt/ZNR/Gox/Nafion) will be discussed during the conference.

Keywords: biosensors, defects, KMnO4, ZnO nanorods

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Authors: N. Prabavathy, R. Balasundaraprabhu, S. Shalini, Dhayalan Velauthapillai, S. Prasanna, N. Muthukumarasamy

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Dye sensitized solar cell (DSSC) has become a significant research area due to their fundamental and scientific importance in the area of energy conversion. Synthetic dyes as sensitizer in DSSC are efficient and durable but they are costlier, toxic and have the tendency to degrade. Natural sensitizers contain plant pigments such as anthocyanin, carotenoid, flavonoid, and chlorophyll which promote light absorption as well as injection of charges to the conduction band of TiO2 through the sensitizer. But, the efficiency of natural dyes is not up to the mark mainly due to instability of the pigment such as anthocyanin. The stability issues in vitro are mainly due to the effect of solvents on extraction of anthocyanins and their respective pH. Taking this factor into consideration, in the present work, the anthocyanins were extracted from the flower Caesalpinia pulcherrima (C. pulcherrimma) with various solvents and their respective stability and pH values are discussed. The usage of citric acid as solvent to extract anthocyanin has shown good stability than other solvents. It also helps in enhancing the sensitization properties of anthocyanins with Titanium dioxide (TiO2) nanorods. The IPCE spectra show higher photovoltaic performance for dye sensitized TiO2nanorods using citric acid as solvent. The natural DSSC using citric acid as solvent shows a higher efficiency compared to other solvents. Hence citric acid performs to be a safe solvent for natural DSSC in boosting the photovoltaic performance and maintaining the stability of anthocyanins.

Keywords: Caesalpinia pulcherrima, citric acid, dye sensitized solar cells, TiO₂ nanorods

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Authors: Khaled M. Khleifat

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An extracellular methanol and ethanol tolerant lipase producing bacterial strain K5b4 was isolated from soil samples contaminated with hydrocarbon residues. It was identified by using morphological and biochemical characteristics and 16srRNA technique as Acinetobacter species. The immobilized lipase from Acinetobacter sp. K5b4 retained more than 98% of its residual activity after incubation with pure methanol and ethanol for 24 hours. The highest hydrolytic activity of the immobilized enzyme was obtained in the presence of 75% (v/v) methanol in the assay solution. In contrary, the enzyme was able to maintain its original activity up to only 25% (v/v) ethanol whereas at elevated concentrations of 50 and 75% (v/v) the enzyme activity was reduced to 10 and 40%, respectively. Maximum lipase activity of 31.5 mU/mL was achieved after 48 hr cultivation when the optimized medium (pH 7.0) that composed of 1.0% (w/v) olive oil, 0.2% (w/v) glycerol, 0.15% (w/v) yeast extract, and 0.05% (w/v) NaCl was inoculated with 0.4% (v/v) seed culture and incubated at 30°C and 150 rpm agitation speed. However, the presence of CaCl2 in the growth media did not show any inhibitory or stimulatory effect on the enzyme production as it compared to the control experiment. Meanwhile, the other mineral salts MgCl2, MnCl2, KCl and CoCl2 were negatively affected the production of lipase enzyme. The inhibition of lipase production from Acinetobacter sp. K5b4 in presence of glucose suggesting that lipase gene expression is prone to catabolic repression.

Keywords: K5B4, methanol and ethanol, acinetobacter, morphological

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Authors: Ke-Jing Lee, Cheng-Jung Lee, Yu-Chi Chang, Li-Wen Wang, Yeong-Her Wang

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To avoid the cross-talk issue of only resistive random access memory (RRAM) cell, one transistor and one resistor (1T1R) architecture with a TiO₂-based RRAM cell connected with solution barium zirconate nickelate (BZN) organic thin film transistor (OTFT) device is successfully demonstrated. The OTFT were fabricated on a glass substrate. Aluminum (Al) as the gate electrode was deposited via a radio-frequency (RF) magnetron sputtering system. The barium acetate, zirconium n-propoxide, and nickel II acetylacetone were synthesized by using the sol-gel method. After the BZN solution was completely prepared using the sol-gel process, it was spin-coated onto the Al/glass substrate as the gate dielectric. The BZN layer was baked at 100 °C for 10 minutes under ambient air conditions. The pentacene thin film was thermally evaporated on the BZN layer at a deposition rate of 0.08 to 0.15 nm/s. Finally, gold (Au) electrode was deposited using an RF magnetron sputtering system and defined through shadow masks as both the source and drain. The channel length and width of the transistors were 150 and 1500 μm, respectively. As for the manufacture of 1T1R configuration, the RRAM device was fabricated directly on drain electrodes of TFT device. A simple metal/insulator/metal structure, which consisting of Al/TiO₂/Au structures, was fabricated. First, Au was deposited to be a bottom electrode of RRAM device by RF magnetron sputtering system. Then, the TiO₂ layer was deposited on Au electrode by sputtering. Finally, Al was deposited as the top electrode. The electrical performance of the BZN OTFT was studied, showing superior transfer characteristics with the low threshold voltage of −1.1 V, good saturation mobility of 5 cm²/V s, and low subthreshold swing of 400 mV/decade. The integration of the BZN OTFT and TiO₂ RRAM devices was finally completed to form 1T1R configuration with low power consumption of 1.3 μW, the low operation current of 0.5 μA, and reliable data retention. Based on the I-V characteristics, the different polarities of bipolar switching are found to be determined by the compliance current with the different distribution of the internal oxygen vacancies used in the RRAM and 1T1R devices. Also, this phenomenon can be well explained by the proposed mechanism model. It is promising to make the 1T1R possible for practical applications of low-power active matrix flat-panel displays.

Keywords: one transistor and one resistor (1T1R), organic thin-film transistor (OTFT), resistive random access memory (RRAM), sol-gel

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Authors: V. Marzal, J. C. Torres, B. Garcia-Camara, Manuel Cano-Garcia, Xabier Quintana, I. Perez Garcilopez, J. M. Sanchez-Pena

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At the present time, the use of nanostructures in complex media, like liquid crystals, is widely extended to manipulate their properties, either electrical or optical. In addition, these media can also be used to control the optical properties of the nanoparticles, for instance when they are resonant. In this work, the change on electrical properties of a liquid crystal cell by adding TiO₂ nanoparticles on one of the alignment layers has been analyzed. These nanoparticles, with a diameter of 100 nm and spherical shape, were deposited in one of the substrates (ITO + polyimide) by spin-coating in order to produce a homogeneous layer. These substrates were checked using an optical microscope (objective x100) to avoid potential agglomerates. The liquid crystal cell is then fabricated, using one of these substrates and another without nanoparticles, and filled with E7. The study of the electrical response was done through impedance measurements in a long range of frequencies (3 Hz- 6 MHz) and at ambient temperature. Different nanoparticle concentrations were considered, as well as pure E7 and an empty cell for comparison purposes. Results about the effective dielectric permittivity and conductivity are presented along with models of equivalent electric circuits and its physical interpretation. As a summary, it has been observed the clear influence of the presence of the nanoparticles, strongly modifying the electric response of the device. In particular, a variation of both the effective permittivity and the conductivity of the device have been observed. This result requires a deep analysis of the effect of these nanoparticles on the trapping of free ions in the device, allowing a controlled manipulation and frequency tuning of the electrical response of these devices.

Keywords: alignment layer, electrical behavior, liquid crystal, TiO₂ nanoparticles

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Authors: Wilman Septina, Rajiv R. Prabhakar, Thomas Moehl, David Tilley

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Cupric oxide (CuO) is a promising absorber material for the fabrication of scalable, low cost solar energy conversion devices, due to the high abundance and low toxicity of copper. It is a p-type semiconductor with a band gap of around 1.5 eV, absorbing a significant portion of the solar spectrum. One of the main challenges in using CuO as solar absorber in an aqueous system is its tendency towards photocorrosion, generating Cu2O and metallic Cu. Although there have been several reports of CuO as a photocathode for hydrogen production, it is unclear how much of the observed current actually corresponds to H2 evolution, as the inevitability of photocorrosion is usually not addressed. In this research, we investigated the effect of the deposition of overlayers onto CuO thin films for the purpose of enhancing its photostability as well as performance for water splitting applications. CuO thin film was fabricated by galvanic electrodeposition of metallic copper onto gold-coated FTO substrates, followed by annealing in air at 600 °C. Photoelectrochemical measurement of the bare CuO film using 1 M phosphate buffer (pH 6.9) under simulated AM 1.5 sunlight showed a current density of ca. 1.5 mA cm-2 (at 0.4 VRHE), which photocorroded to Cu metal upon prolonged illumination. This photocorrosion could be suppressed by deposition of 50 nm-thick TiO2, deposited by atomic layer deposition. In addition, we found that insertion of an n-type CdS layer, deposited by chemical bath deposition, between the CuO and TiO2 layers was able to enhance significantly the photocurrent compared to without the CdS layer. A photocurrent of over 2 mA cm-2 (at 0 VRHE) was observed using the photocathode stack FTO/Au/CuO/CdS/TiO2/Pt. Structural, electrochemical, and photostability characterizations of the photocathode as well as results on various overlayers will be presented.

Keywords: CuO, hydrogen, photoelectrochemical, photostability, water splitting

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Authors: Emine Yılmaz, Serap Fındık

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Baker’s yeast industry uses molasses as a raw material. Molasses is end product of sugar industry. Wastewater from molasses processing presents large amount of coloured substances that give dark brown color and high organic load to the effluents. The main coloured compounds are known as melanoidins. Melanoidins are product of Maillard reaction between amino acid and carbonyl groups in molasses. Dark colour prevents sunlight penetration and reduces photosynthetic activity and dissolved oxygen level of surface waters. Various methods like biological processes (aerobic and anaerobic), ozonation, wet air oxidation, coagulation/flocculation are used to treatment of baker’s yeast effluent. Before effluent is discharged adequate treatment is imperative. In addition to this, increasingly stringent environmental regulations are forcing distilleries to improve existing treatment and also to find alternative methods of effluent management or combination of treatment methods. Sonochemical oxidation is one of the alternative methods. Sonochemical oxidation employs ultrasound resulting in cavitation phenomena. In this study, decolorization of baker’s yeast effluent was investigated by using ultrasound. Baker’s yeast effluent was supplied from a factory which is located in the north of Turkey. An ultrasonic homogenizator used for this study. Its operating frequency is 20 kHz. TiO2-ZnO catalyst has been used as sonocatalyst. The effects of molar proportion of TiO2-ZnO, calcination temperature and time, catalyst amount were investigated on the decolorization of baker’s yeast effluent. The results showed that prepared composite TiO2-ZnO with 4:1 molar proportion treated at 700°C for 90 min provides better result. Initial decolorization rate at 15 min is 3% without catalyst, 14,5% with catalyst treated at 700°C for 90 min respectively.

Keywords: baker’s yeast effluent, decolorization, sonocatalyst, ultrasound

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Authors: Prasanta Sutradhar, Mitali Saha

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With an increasing awareness of green and clean energy, zinc oxide based solar cells were found to be suitable candidates for cost-effective and environmentally friendly energy conversion devices. In this work, we have reported the green synthesis of zinc oxide nanoparticles (ZnO) by thermal method and under microwave irradiation using the aqueous extract of tomatoes as non-toxic and ecofriendly reducing material. The synthesized ZnO nanoparticles were characterised by UV-Visible spectroscopy (UV-Vis), infra-red spectroscopy (IR), particle size analyser (DLS), scanning electron microscopy (SEM), atomic force microscopy (AFM), and X- ray diffraction study (XRD). A series of ZnO nanocomposites with titanium dioxide nanoparticles (TiO2) and graphene oxide (GO) were prepared for photovoltaic application. Structural and morphological studies of these nanocomposites were carried out using UV-vis, SEM, XRD, and AFM. The current-voltage measurements of the nanocomposites demonstrated enhanced power conversion efficiency of 6.18% in case of ZnO/GO/TiO2 nanocomposite.

Keywords: ZnO, green synthesis, microwave, nanocomposites, I-V characteristics

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Authors: Refal Hussain, Saifuddin M. Nomanbhay

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Glycerol is a valuable raw material for the production of industrially useful metabolites. Among many promising applications for the use of glycerol is its bioconversion to high value-added compounds, such as bioethanol through microbial fermentation. Bioethanol is an important industrial chemical with emerging potential as a biofuel to replace vanishing fossil fuels. The yield of liquid fuel in this process was greatly influenced by various parameters viz, temperature, pH, glycerol concentration, organic concentration, and agitation speed were considered. The present study was undertaken to investigate optimum parameters for bioethanol production from raw glycerol by immobilized mutant Escherichia coli (E.coli) (ATCC11505) strain on chitosan cross linked glutaraldehyde optimized by Taguchi statistical method in shake flasks. The initial parameters were set each at four levels and the orthogonal array layout of L16 (45) conducted. The important controlling parameters for optimized the operational fermentation was temperature 38 °C, medium pH 6.5, initial glycerol concentration (250 g/l), and organic source concentration (5 g/l). Fermentation with optimized parameters was carried out in a custom fabricated shake flask. The predicted value of bioethanol production under optimized conditions was (118.13 g/l). Immobilized cells are mainly used for economic benefits of continuous production or repeated use in continuous as well as in batch mode.

Keywords: bioethanol, Escherichia coli, immobilization, optimization

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Authors: J. Tirano, H. Zea, C. Luhrs

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It is well known that titanium dioxide is a semiconductor with several applications in photocatalytic process. Its band gap makes it very interesting in the photoelectrodes manufacturing used in photoelectrochemical cells for hydrogen production, a clean and environmentally friendly fuel. The synthesis of 1D titanium dioxide nanostructures, such as nanotubes, makes possible to produce more efficient photoelectrodes for solar energy to hydrogen conversion. In essence, this is because it increases the charge transport rate, decreasing recombination options. However, its principal constraint is to be mainly sensitive to UV range, which represents a very low percentage of solar radiation that reaches earth's surface. One of the alternatives to modifying the TiO2’s band gap and improving its photoactivity under visible light irradiation is to dope the nanotubes with transition metals. This option requires fabricating efficient nanostructured photoelectrodes with controlled morphology and specific properties able to offer a suitable surface area for metallic doping. Hence, currently one of the central challenges in photoelectrochemical cells is the construction of nanomaterials with a proper band position for driving the reaction while absorbing energy over the VIS spectrum. This research focuses on the synthesis and characterization of Nidoped TiO2 nanotubes for improving its photocatalytic activity in solar energy conversion applications. Initially, titanium dioxide nanotubes (TNTs) with controlled morphology were synthesized by two-step potentiostatic anodization of titanium foil. The anodization was carried out at room temperature in an electrolyte composed of ammonium fluoride, deionized water and ethylene glycol. Consequent thermal annealing of as-prepared TNTs was conducted in the air between 450 °C - 550 °C. Afterwards, the nanotubes were superficially modified by nickel deposition. Morphology and crystalline phase of the samples were carried out by SEM, EDS and XRD analysis before and after nickel deposition. Determining the photoelectrochemical performance of photoelectrodes is based on typical electrochemical characterization techniques. Also, the morphological characterization associated electrochemical behavior analysis were discussed to establish the effect of nickel nanoparticles modification on the TiO2 nanotubes. The methodology proposed in this research allows using other transition metal for nanotube surface modification.

Keywords: dimensionally stable electrode, nickel nanoparticles, photo-electrode, TiO₂ nanotubes

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Authors: Mohannad Mayyas, Farshid Pahlevani, Veena Sahajwalla

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Automotive shredder residue (ASR) is an industrial waste, generated during the recycling process of End-of-life vehicles. The large increasing production volumes of ASR and its hazardous content have raised concerns worldwide, leading some countries to impose more restrictions on ASR waste disposal and encouraging researchers to find efficient solutions for ASR processing. Although a great deal of research work has been carried out, all proposed solutions, to our knowledge, remain commercially and technically unproven. While the volume of waste materials continues to increase, the production of materials from new sustainable sources has become of great importance. Advanced ceramic materials such as nitrides, carbides and borides are widely used in a variety of applications. Among these ceramics, a great deal of attention has been recently paid to Titanium nitride (TiN) owing to its unique characteristics. In our study, we propose a new sustainable approach for ASR management where TiN nanoparticles with ideal particle size ranging from 200 to 315 nm can be synthesized as a by-product. In this approach, TiN is thermally synthesized by nitriding pressed mixture of automotive shredder residue (ASR) incorporated with titanium oxide (TiO2). Results indicated that TiO2 influences and catalyses degradation reactions of ASR and helps to achieve fast and full decomposition. In addition, the process resulted in titanium nitride (TiN) ceramic with several unique structures (porous nanostructured, polycrystalline, micro-spherical and nano-sized structures) that were simply obtained by tuning the ratio of TiO2 to ASR, and a product with appreciable TiN content of around 85% was achieved after only one hour nitridation at 1550 °C.

Keywords: automotive shredder residue, nano-ceramics, waste treatment, titanium nitride, thermal conversion

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Authors: Chundong Li, V. V. Neshchimenko, M. M. Mikhailov

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The effect of the modification of ZnO powders by ZrO2, Al2O3, TiO2, SiO2, CeO2 and Y2O3 nanoparticles with a concentration of 1-30 wt % is investigated by diffuse reflectance spectra within the wavelength range 200 to 2500 nm before and after 100 keV proton and electron irradiation. It has been established that the introduction of nanoparticles ZrO2, Al2O3 enhances the optical stability of the pigments under proton irradiation, but reduces it under electron irradiation. Modifying with TiO2, SiO2, CeO2, Y2O3 nanopowders leads to decrease radiation stability in both types of irradiation. Samples modified by 5 wt. % of ZrO2 nanoparticles have the highest stability of optical properties after proton exposure. The degradation of optical properties under electron irradiation is not high for this concentration of nanoparticles. A decrease in the absorption of pigments modified with nanoparticles proton exposure is determined by a decrease in the intensity of bands located in the UV and visible regions. After electron exposure the absorption bands have in the whole spectrum range.

Keywords: irradiation, nanopowders, radiation stability, zinc oxide

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Authors: Malek Y. S. Ibrahim, Jeffrey A. Bennett, Milad Abolhasani

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Despite the potential of hydrogen (H2) storage in liquid organic carriers to achieve carbon neutrality, the energy required for H2 release and the cost of catalyst recycling has hindered its large-scale adoption. In response, a photo flow reactor packed with rhodium (Rh)/titania (TiO2) photocatalyst was reported for the continuous and selective acceptorless dehydrogenation of 1,2,3,4-tetrahydroquinoline to H2 gas and quinoline under visible light irradiation at room temperature. The tradeoff between the reactor pressure drop and its photocatalytic surface area was resolved by selective in-situ photodeposition of Rh in the photo flow reactor post-packing on the outer surface of the TiO2 microparticles available to photon flux, thereby reducing the optimal Rh loading by 10 times compared to a batch reactor, while facilitating catalyst reuse and regeneration. An example of using quinoline as a hydrogen acceptor to lower the energy of the hydrogen production step was demonstrated via the water-gas shift reaction.

Keywords: hydrogen storage, flow chemistry, photocatalysis, solar hydrogen

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Authors: Vijay K. Tomer, Ritu Malik, Satya P. Nehra, Anshu Sharma

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Highly ordered mesoporous WO₃-TiO₂ nanohybrids with large intrinsic surface area and highly ordered pore channels were synthesized using mesoporous silica, KIT-6 as hard template using a nanocasting strategy. The nanohybrid samples were characterized by a variety of physico-chemical techniques including X-ray diffraction, Nitrogen adsorption-desorption isotherms, and high resolution transmission electron microscope. The nanohybrids were tested for detection of important indoor Volatile Organic Compounds (VOCs) including acetone, ethanol, n-butanol, toluene, and xylene. The sensing result illustrates that the nanocomposite sensor was highly responsive towards xylene gas at relatively lower operating temperature. A rapid response and recovery time, highly linear response and excellent stability in the concentration ranges from 1 to 100 ppm was observed for xylene gas. It is believed that the promising results of this study can be utilized in the synthesis of ordered mesoporous nanostructures which can extend its configuration for the development of new age e-nose type sensors with enhanced gas-sensing performance.

Keywords: nanohybrids, response, sensor, VOCs, xylene

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Authors: Jaejin Han, Jinsub Choi

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Vanadium redox flow battery (VRFB) is a type of redox flow battery which uses vanadium ionic solution as electrolyte. Inside the VRFB, 2.5mm thickness of graphite is generally used as bipolar plate for anti-corrosion of current collector. In this research, thick graphite bipolar plate was substituted by 0.126mm thickness of dimensionally stable anode which was coated with IrO2 on an anodic nanotubular TiO2 substrate. It can provide dimensional advantage over the conventional graphite when the VRFB is used as multi-stack. Ir was coated by using spray coating method in order to enhance electric conductivity. In this study, various electrochemical characterizations were carried out. Cyclic voltammetry data showed activation of Ir in the positive electrode of VRFB. In addition, polarization measurements showed Ir-coated DSA had low overpotential in the positive electrode of VRFB. In cell test results, the DSA-used VRFB showed better efficiency than graphite-used VRFB in voltage and overall efficiency.

Keywords: bipolar plate, DSA (dimensionally stable anode), iridium oxide coating, TiO2 nanotubes, VRFB (vanadium redox flow battery)

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Authors: Bouafia-Chergui Souâd, Chabani Malika, Bensmaili Aicha

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Water treatment and especially, medicament pollutants are nowadays important problems. Degradation of oxytetracycline was carried out using combined process of low-frequency ultrasound (US), ultraviolet irradiation and a catalyst. The effectiveness of the coupled processes has been evaluated by studying the effects of various operating parameters including initial OTC concentration, solution pH and catalyst mass. For the photolysis process, the monochromatic ultraviolet light wavelength utilized was 365 nm. The sonolysis experiments were performed with ultrasound at a frequency of 40 kHz. The heterogeneous photocatalysis was studied in the presence of TiO2. The processes were employed individually, and simultaneously to examine the details of the processes and to investigate the contribution of each process. Low UV intensity (12W), low pH and high mass of TiO2 conditions enhanced the sono-photocatalytic degradation of OTC. The results showed that the individual contribution sonochemical and photochemical reactions are very low, however, their coupling increases the degradation rate of 8 times compared to photolysis and 2 times compared to sonolysis. There is a synergistic effect between the two modes of radiation, UV and U.S. leading to 82.04% degradation yield. An application of these combined processes on the treatment of a real pharmaceutical wastewater was examined.

Keywords: sonolysis, photocatalysis, combined process, antibiotic

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Authors: Marcin Debowski, Marcin Zielinski, Miroslaw Krzemieniewski, Agata Glowacka-Gil, Paulina Rusanowska, Magdalena Zielinska, Agnieszka Cydzik-Kwiatkowska

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Technologies of biogas upgrading are now perceived as competitive solution combustion and production of electricity and heat. Biomethane production will ensure broader application as energy carrier than biogas. Biomethane can be used as fuel in internal combustion engines or introduced into the natural gas transmission network. Therefore, there is a need to search for innovative, economically and technically justified methods for biogas enrichment. The aim of this paper is to present a technology solution for biogas upgrading with immobilized algae biomass. Reactor for biogas upgrading with immobilized algae biomass can be used for removing CO₂ from the biogas, flue gases and the waste gases especially coming from different industry sectors, e.g. from the food industry from yeast production process, biogas production systems, liquid and gaseous fuels combustion systems, hydrocarbon processing technology. The basis for the technological assumptions of presented technology were laboratory works and analyses that tested technological variants of biogas upgrading. The enrichment of biogas with a methane content of 90-97% pointed to technological assumptions for installation on a technical scale. Reactor for biogas upgrading with algae biomass is characterized by a significantly lower cubature in relation to the currently used solutions which use CO₂ removal processes. The invention, by its structure, assumes achieving a very high concentration of biomass of algae through its immobilization in capsules. This eliminates the phenomenon of lowering the pH value, i.e. acidification of the environment in which algae grow, resulting from the introduction of waste gases at a high CO₂ concentration. The system for introducing light into algae capsules is characterized by a higher degree of its use, due to lower losses resulting from the phenomenon of absorption of light energy by water. The light from the light source is continuously supplied to the formed biomass of algae or cyanobacteria in capsules by the light tubes. The light source may be sunlight or a light generator of a different wavelength of light from 300 nm to 800 nm. A portion of gas containing CO₂, accumulated in the tank and conveyed by the pump is periodically introduced into the housing of the photobioreactor tank. When conveying the gas that contains CO₂, it penetrates the algal biomass in capsules through the outer envelope, displacing, from the algal biomass, gaseous metabolic products which are discharged by the outlet duct for gases. It contributes to eliminating the negative impact of this factor on CO₂ binding processes. As a result of the cyclic dosing of gases containing carbon dioxide, gaseous metabolic products of algae are displaced and removed outside the technological system. Technology for biogas upgrading with immobilized algae biomass is suitable for the small biogas plant. The advantages of this technology are high efficiency as well as useful algae biomass which can be used mainly as animal feed, fertilizers and in the power industry. The construction of the device allows effective removal of carbon dioxide from gases at a high CO₂ concentration.

Keywords: biogas, carbon dioxide, immobilised biomass, microalgae, upgrading

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Authors: Olga Długosz, Jolanta Pulit-Prociak, Marcin Banach

Abstract:

The paper presents a process to obtain glutathione-modified titanium oxide nanoparticles. The processes were carried out in a microwave radiation field. The influence of the molar ratio of glutathione to titanium oxide and the effect of the fold of NaOH vs. stoichiometric amount on the size of the formed TiO₂ nanoparticles was determined. The physicochemical properties of the obtained products were evaluated using dynamic light scattering (DLS), transmission electron microscope- energy-dispersive X-ray spectroscopy (TEM-EDS), low-temperature nitrogen adsorption method (BET), X-Ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) microscopy methods. The size of TiO₂ nanoparticles was characterized from 30 to 336 nm. The release of titanium ions from the prepared products was evaluated. These studies were carried out using different media in which the powders were incubated for a specific time. These were water, SBF and Ringer's solution. The release of titanium ions from modified products is weaker compared to unmodified titanium oxide nanoparticles. The reduced release of titanium ions may allow the use of such modified materials as substances in drug delivery systems.

Keywords: titanium dioxide, nanoparticles, drug carrier, glutathione

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Authors: Olga Długosz, Jolanta Pulit-Prociak, Marcin Banach

Abstract:

The paper presents a process to obtain glutathione-modified titanium oxide nanoparticles. The processes were carried out in a microwave radiation field. The influence of the molar ratio of glutathione to titanium oxide and the effect of the fold of NaOH vs. stoichiometric amount on the size of the formed TiO₂ nanoparticles was determined. The physicochemical properties of the obtained products were evaluated using dynamic light scattering (DLS), transmission electron microscope- energy-dispersive X-ray spectroscopy (TEM-EDS), low-temperature nitrogen adsorption method (BET), X-Ray Diffraction (XRD), and Fourier-transform infrared spectroscopy (FTIR) microscopy methods. The size of TiO₂ nanoparticles was characterized from 30 to 336 nm. The release of titanium ions from the prepared products was evaluated. These studies were carried out using different media in which the powders were incubated for a specific time. These were: water, SBF, and Ringer's solution. The release of titanium ions from modified products is weaker compared to unmodified titanium oxide nanoparticles. The reduced release of titanium ions may allow the use of such modified materials as substances in drug delivery systems.

Keywords: titanium dioxide, nanoparticles, drug carrier, glutathione

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Authors: Suzanne Giasson, Alberto Guerron

Abstract:

Stimuli-responsive polymer coatings can be used as functional elements in nanotechnologies, such as valves in microfluidic devices, as membranes in biomedical engineering, as substrates for the culture of biological tissues or in developing nanomaterials for targeted therapies in different diseases. However, such coatings usually suffer from major shortcomings, such as a lack of selectivity and poor environmental stability. The study will present multi-responsive hierarchical and hybrid polymer-based coatings aiming to overcome some of these limitations. Hierarchical polymer coatings, consisting of two-dimensional arrays of thermo-responsive cationic PNIPAM-based microgels and surface-functionalized with non-responsive or pH-responsive polymers, were covalently grafted to substrates to tune the surface chemistry and the elasticity of the surface independently using different stimuli. The characteristic dimensions (i.e., layer thickness) and surface properties (i.e., adhesion, friction) of the microgel coatings were assessed using the Surface Forces Apparatus. The ability to independently control the swelling and surface properties using temperature and pH as triggers were investigated for microgels in aqueous suspension and microgels immobilized on substrates. Polymer chain grafting did not impede the ability of cationic PNIPAM microgels to undergo a volume phase transition above the VPTT, either in suspension or immobilized on a substrate. Due to the presence of amino groups throughout the entirety of the microgel polymer network, the swelling behavior was also pH dependent. However, the thermo-responsive swelling was more significant than the pH-triggered one. The microgels functionalized with PEG exhibited the most promising behavior. Indeed, the thermo-triggered swelling of microgel-co-PEG did not give rise to changes in the microgel surface properties (i.e., surface potential and adhesion) within a wide range of pH values. It was possible for the immobilized microgel-co-PEG to undergo a volume transition (swelling/shrinking) with no change in adhesion, suggesting that the surface of the thermal-responsive microgels remains rather hydrophilic above the VPTT. This work confirms the possibility of tuning the swelling behavior of microgels without changing the adhesive properties. Responsive surfaces whose swelling properties can be reversibly and externally altered over space and time regardless of the surface chemistry are very innovative and will enable revolutionary advances in technologies, particularly in biomedical surface engineering and microfluidics, where advanced assembly of functional components is increasingly required.

Keywords: responsive materials, polymers, surfaces, cell culture

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Authors: D. Olszewska, J. Niewiedzial

Abstract:

In some types of Li-ion batteries carbon in the form of graphite is used. Unfortunately, carbon materials, in particular graphite, have very good electrochemical properties, but increase their volume during charge/discharge cycles, which may even lead to an explosion of the cell. The cell element may be replaced by a composite material consisting of lithium-titanium oxide Li4Ti5O12 (LTO) modified with copper and nickel ions and carbon derived from sucrose. This way you can improve the conductivity of the material. LTO is appropriate only for applications which do not require high energy density because of its high operating voltage (ca. 1.5 V vs. Li/Li+). Specific capacity of Li4Ti5O12 is high enough for utilization in Li-ion batteries (theoretical capacity 175 mAh·g-1) but it is lower than capacity of graphite anodes. Materials based on Li4Ti5O12 do not change their volume during charging/discharging cycles, however, LTO has low conductivity. Another positive aspect of the use of sucrose in the carbon composite material is to eliminate the addition of carbon black from the anode of the battery. Therefore, the proposed materials contribute significantly to environmental protection and safety of selected lithium cells. New anode materials in order to obtain Li3.8Cu0.1Ni0.1Ti5O12 have been prepared by solid state synthesis using three-way: i) stoichiometric composition of Li2CO3, TiO2, CuO, NiO (A- Li3.8Cu0.1Ni0.1Ti5O12); ii) stoichiometric composition of Li2CO3, TiO2, Cu(NO3)2, Ni(NO3)2 (B-Li3.8Cu0.1Ni0.1Ti5O12); and iii) stoichiometric composition of Li2CO3, TiO2, CuO, NiO calcined with 10% of saccharose (Li3.8Cu0.1Ni0.1Ti5O12-C). Structure of materials was studied by X-ray diffraction (XRD). The electrochemical properties were performed using appropriately prepared cell Li|Li+|Li3.8Cu0.1Ni0.1Ti5O12 for cyclic voltammetry and discharge/charge measurements. The cells were periodically charged and discharged in the voltage range from 1.3 to 2.0 V applying constant charge/discharge current in order to determine the specific capacity of each electrode. Measurements at various values of the charge/discharge current (from C/10 to 5C) were carried out. Cyclic voltammetry investigation was carried out by applying to the cells a voltage linearly changing over time at a rate of 0.1 mV·s-1 (in the range from 2.0 to 1.3 V and from 1.3 to 2.0 V). The XRD method analyzes show that composite powders were obtained containing, in addition to the main phase, 4.78% and 4% TiO2 in A-Li3.8Cu0.1Ni0.1O12 and B-Li3.8Cu0.1Ni0.1O12, respectively. However, Li3.8Cu0.1Ni0.1O12-C material is three-phase: 63.84% of the main phase, 17.49 TiO2 and 18.67 Li2TiO3. Voltammograms of electrodes containing materials A-Li3.8Cu0.1Ni0.1O12 and B-Li3.8Cu0.1Ni0.1O12 are correct and repeatable. Peak cathode occurs for both samples at a potential approx. 1.52±0.01 V relative to a lithium electrode, while the anodic peak at potential approx. 1.65±0.05 V relative to a lithium electrode. Voltammogram of Li3.8Cu0.1Ni0.1Ti5O12-C (especially for the first measurement cycle) is not correct. There are large variations in values of specific current, which are not characteristic for materials LTO. From the point of view of safety and environmentally friendly production of Li-ion cells eliminating soot and applying Li3.8Cu0.1Ni0.1Ti5O12-C as an active material of an anode in lithium-ion batteries seems to be a good alternative to currently used materials.

Keywords: anode, Li-ion batteries, Li₄O₅O₁₂, spinel

Procedia PDF Downloads 128

Authors: Eka Maulana, Sholeh Hadi Pramono, Dody Fanditya, M. Julius

Abstract:

In this paper, extract of papaya leaves are used as a natural dye and combined by variations of solvent concentration applied on DSSC (Dye-Sensitized Solar Cell). Indonesian geographic located on the equator line occasions the magnitude of the potential to develop organic solar cells made from extracts of chlorophyll as a substitute for inorganic materials or synthetic dye on DSSC material. Dye serves as absorbing photons which are then converted into electrical energy. A conductive coated glass layer called TCO (Transparent Conductive Oxide) is used as a substrate of electrode. TiO2 nanoparticles as binding dye molecules, redox couple iodide/ tri-iodide as the electrolyte and carbon as the counter electrode in the DSSC are used. TiO2 nanoparticles, organic dyes, electrolytes and counter electrode are arranged and combined with the layered structure of the photo-catalyst absorption layer. Dye absorption measurements using a spectrophotometer at 200-800 nm light spectrum produces a total amount of chlorophyll 80.076 mg/l. The test cell at 7 watt LED light with 5000 lux luminescence were obtained Voc and Isc of 235.5 mV and 14 μA, respectively.

Keywords: DSSC (Dye-Sensitized Solar Cell), natural dye, chlorophyll, absorption

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Authors: Heba M. Gobara, Ahmed A. M. El-Naggar, Rasha S. El-Sayed, Amal A. AlKahlawy

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In this study, metal organic framework (Cr-MIL-101) and TiO₂ nanoparticles were utilized as two semiconductors for water splitting process. The coupling of both semiconductors in order to improve the photocatalytic reactivity for the hydrogen production in presence of methanol as a hole scavenger under visible light (sunlight) has been performed. The forementioned semiconductors and the collected samples after water splitting application are characterized by several techniques viz., XRD, N₂ adsorption-desorption, TEM, ED, EDX, Raman spectroscopy and the total content of carbon. The results revealed an efficient yield of H₂ production with maximum purity 99.3% with the in-situ formation of graphene oxide nanosheets and multiwalled carbon nanotubes coated over the surface of the physically mixed Cr-MIL-101–TiO₂ system. The amount of H₂ gas produced was stored when using Cr-MIL-101 catalyst individually. The obtained data in this work provides promising candidate materials for pure hydrogen production as a clean fuel acquired from the water splitting process. In addition, the in-situ production of graphene nanosheets and carbon nanotubes is counted as promising advances for the presented process.

Keywords: hydrogen production, water splitting, photocatalysts, Graphene

Procedia PDF Downloads 156

Authors: Harikrishna Yadav Nanganuru, Narasimhulu Korrapati

Abstract:

The demand for the lead (Pb) in the battery industry has been growing for last twenty years. On an average about 2.35 million tons of lead is used in the battery industry. According to the survey of supply and demand battery industry is using 75% of lead produced every year. Due to the increase in battery scrap, secondary lead production has been increasing in this decade. Europe and USA together account for 75% of the world’s secondary lead production. The effluent from used battery scrap consists of high concentrations of lead. Unauthorized disposal of spent batteries, which contain intolerable concentration of lead, into landfills or municipal water canals causes release of Pb into the environment. Lead is one of the toxic heavy metals that have large damaging effects on the human health. Due to its persistence and toxicity, the presence of Pb in drinking water is considered as a special concern. Accumulation of Pb in the human body for long period of time can result in the malfunctioning of some organs. Many technologies have been developed for the removal of lead using microorganisms. In this paper, effluent was taken from the spent battery scrap and was characterized by inductively coupled plasma atomic emission spectrometer. Microorganisms play an important role in removal of lead from the contaminated sites. So, the bacteria were isolated from the effluent. Optimum conditions for the microbial growth and applied for the lead removal. These bacterial cells were immobilized and used for the removal of Pb from the known concentration of metal solution. Scanning electron microscopic (SEM) studies were shown that the Pb was efficiently adsorbed by the immobilized bacteria. From the results of Atomic Absorption Spectroscopy (AAS), 83.40 percentage of Pb was removed in a batch culture.

Keywords: adsorption, effluent, immobilization, lead (Pb)

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Authors: Aliaa M. El-Borai, Ehab A. Beltagy, Eman E. Gadallah, Samy A. ElAssar

Abstract:

Bioremediation technology is now used for treatment instead of traditional metal removal methods. A strain was isolated from Marsa Alam, Red sea, Egypt showed high resistance to high lead concentration and was identified by the 16S rRNA gene sequencing technique as Halomonas sp. ES015. Medium optimization was carried out using Plackett-Burman design, and the most significant factors were yeast extract, casamino acid and inoculums size. The optimized media obtained by the statistical design raised the removal efficiency from 84% to 99% from initial concentration 250 ppm of lead. Moreover, Box-Behnken experimental design was applied to study the relationship between yeast extract concentration, casamino acid concentration and inoculums size. The optimized medium increased removal efficiency to 97% from initial concentration 500 ppm of lead. Immobilized Halomonas sp. ES015 cells on sponge cubes, using optimized medium in loop bioremediation column, showed relatively constant lead removal efficiency when reused six successive cycles over the range of time interval. Also metal removal efficiency was not affected by flow rate changes. Finally, the results of this research refer to the possibility of lead bioremediation by free or immobilized cells of Halomonas sp. ES015. Also, bioremediation can be done in batch cultures and semicontinuous cultures using column technology.

Keywords: bioremediation, lead, Box–Behnken, Halomonas sp. ES015, loop bioremediation, Plackett-Burman

Procedia PDF Downloads 166

Authors: Zainab Dahrouch, Beatrix Petrovičová, Claudia Triolo, Fabiola Pantò, Angela Malara, Salvatore Patanè, Maria Allegrini, Saveria Santangelo

Abstract:

Synthetic dyes dispersed in water cause environmental damage and have harmful effects on human health. Methylene blue (MB) is broadly used as a dye in the textile, pharmaceutical, printing, cosmetics, leather, and food industries. The complete removal of MB is difficult due to the presence of aromatic rings in its structure. The present study is focused on electrospun nanofibers (NFs) with engineered architecture and surface to be used as catalysts for the photodegradation of MB. Ti and/or Zn oxide NFs are produced by electrospinning precursor solutions with different Ti: Zn molar ratios (from 0:1 to 1:0). Subsequent calcination and cooling steps are operated at fast rates to generate porous NFs with capture centers to reduce the recombination rate of the photogenerated charges. The comparative evaluation of the NFs as photocatalysts for the removal of MB from an aqueous solution with a dye concentration of 15 µM under UV irradiation shows that the binary (wurtzite ZnO and anatase TiO₂) oxides exhibit higher catalytic activity compared to ternary (ZnTiO₃ and Zn₂TiO₄) oxides. The higher band gap and lower crystallinity of the ternary oxides are responsible for their lower photocatalytic activity. It has been found that the optimal load for the wurtzite ZnO is 0.66 mg mL⁻¹, obtaining a degradation rate of 7.94.10⁻² min⁻¹. The optimal load for anatase TiO₂ is lower (0.33 mg mL⁻¹) and the corresponding rate constant (1.12×10⁻¹ min⁻¹) is higher. This finding (higher activity with lower load) is of crucial importance for the scaling up of the process on an industrial scale. Indeed, the anatase NFs outperform even the commonly used P25-TiO₂ benchmark. Besides, they can be reused twice without any regeneration treatment, with 5.2% and 18.7% activity decrease after second and third use, respectively. Thanks to the scalability of the electrospinning technique, this laboratory-scale study provides a perspective towards the sustainable large-scale manufacture of photocatalysts for the treatment of industry effluents.

Keywords: anatase, capture centers, methylene blue dye, nanofibers, photodegradation, zinc oxide

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Authors: Anahita Mortazavi Manesh, Mojtaba Bagherzadeh

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Metalloporphyrins are well known to mimic the activity of monooxygenase enzymes. In this regard, metalloporphyrin complexes have been largely employed as valuable biomimetic catalysts, owing to the critical roles they play in oxygen transfer processes in catalytic oxidation reactions. Investigating in this area is based on different strategies to design selective, stable and high turnover catalytic systems. Immobilization of expensive metalloporphyrin catalysts onto supports appears to be a good way to improve their stability, selectivity and the catalytic performance because of the support environment and other advantages with respect to recovery, reuse. In other words, supporting metalloporphyrins provides a physical separation of active sites, thus minimizing catalyst self-destruction and dimerization of unhindered metalloporphyrins. Furthermore, heterogeneous catalytic oxidations have become an important target since their process are used in industry, helping to minimize the problems of industrial waste treatment. Hence, the immobilization of these biomimetic catalysts is much desired. An attractive approach is the preparation of the heterogeneous catalyst involves immobilization of complexes on silica coated magnetic nano-particles. Fe3O4@SiO2 magnetic nanoparticles have been studied extensively due to their superparamagnetism property, large surface area to volume ratio and easy functionalization. Using heterogenized homogeneous catalysts is an attractive option to facile separation of catalyst, simplified product work-up and continuity of catalytic system. Homogeneous catalysts immobilized on magnetic nanoparticles (MNPs) surface occupy a unique position due to combining the advantages of both homogeneous and heterogeneous catalysts. In addition, superparamagnetic nature of MNPs enable very simple separation of the immobilized catalysts from the reaction mixture using an external magnet. In the present work, an efficient heterogeneous catalyst was prepared by immobilizing manganese porphyrin on functionalized magnetic nanoparticles through the amino propyl linkage. The prepared catalyst was characterized by elemental analysis, FT-IR spectroscopy, X-ray powder diffraction, atomic absorption spectroscopy, UV-Vis spectroscopy, and scanning electron microscopy. Application of immobilized metalloporphyrin in the oxidation of various organic substrates was explored using Gas chromatographic (GC) analyses. The results showed that the supported Mn-porphyrin catalyst (Fe3O4@SiO2-NH2@MnPor) is an efficient and reusable catalyst in oxidation reactions. Our catalytic system exhibits high catalytic activity in terms of turnover number (TON) and reaction conditions. Leaching and recycling experiments revealed that nanocatalyst can be recovered several times without loss of activity and magnetic properties. The most important advantage of this heterogenized catalytic system is the simplicity of the catalyst separation in which the catalyst can be separated from the reaction mixture by applying a magnet. Furthermore, the separation and reuse of the magnetic Fe3O4 nanoparticles were very effective and economical.

Keywords: Fe3O4 nanoparticle, immobilized metalloporphyrin, magnetically separable nanocatalyst, oxidation reactions

Procedia PDF Downloads 274