Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 12528

Search results for: hydrothermal process

12528 Vertically Grown P–Type ZnO Nanorod on Ag Thin Film

Authors: Jihyun Park, Tae Il Lee, Jae-Min Myoung


A Silver (Ag) thin film is introduced as a template and doping source for vertically aligned p–type ZnO nanorods. ZnO nanorods were grown using a ammonium hydroxide based hydrothermal process. During the hydrothermal process, the Ag thin film was dissolved to generate Ag ions in the solution. The Ag ions can contribute to doping in the wurzite structure of ZnO and the (111) grain of Ag thin film can be the epitaxial temporal template for the (0001) plane of ZnO. Hence, Ag–doped p–type ZnO nanorods were successfully grown on the substrate, which can be an electrode or semiconductor for the device application. To demonstrate the potentials of this idea, p–n diode was fabricated and its electrical characteristics were demonstrated.

Keywords: hydrothermal process, Ag–doped ZnO nanorods, p–type ZnO

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12527 Comparison of Methods for the Synthesis of Eu+++, Tb+++, and Tm+++ Doped Y2O3 Nanophosphors by Sol-Gel and Hydrothermal Methods for Bioconjugation

Authors: Ravindra P. Singh, Drupad Ram, Dinesh K. Gupta


Rare earth ions doped metal oxides are a class of luminescent materials which have been proved to be excellent for applications in field emission displays and cathode ray tubes, plasma display panels. Under UV irradiation Eu+++ doped Y2O3 is a red phosphor and Tb+++ doped Y 2O3 is a green phosphor. It is possible that, due to their high quantum efficiency, they might serve as improved luminescent markers for identification of biomolecules, as already reported for CdSe and CdSe/ZnS nanocrystals. However, for any biological applications these particle powders must be suspended in water while retaining their phosphorescence. We hereby report synthesis and characterization of Eu+++ and Tb+++ doped yttrium oxide nanoparticles by sol-gel and hydrothermal processes. Eu+++ and Tb+++ doped Y2O3 nanoparticles have been synthesized by hydrothermal process using yttrium oxo isopropoxide [Y5O(OPri)13] (crystallized twice) and it’s acetyl acetone modified product [Y(O)(acac)] as precursors. Generally the sol-gel derived metal oxides are required to be annealed to the temperature ranging from 400°C-800°C in order to develop crystalline phases. However, this annealing also results in the development of aggregates which are undesirable for bio-conjugation experiments. In the hydrothermal process, we have achieved crystallinity of the nanoparticles at 300°C and the development of crystalline phases has been found to be proportional to the time of heating of the reactor. The average particle sizes as calculated from XRD were found to be 28 nm, 32 nm, and 34 nm by hydrothermal process. The particles were successfully suspended in chloroform in the presence of trioctyl phosphene oxide and TEM investigations showed the presence of single particles along with agglomerates.

Keywords: nanophosphors, Y2O3:Eu+3, Y2O3:Tb+3, sol-gel, hydrothermal method, TEM, XRD

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12526 Algae for Wastewater Treatment and CO₂ Sequestration along with Recovery of Bio-Oil and Value Added Products

Authors: P. Kiran Kumar, S. Vijaya Krishna, Kavita Verma1, V. Himabindu


Concern about global warming and energy security has led to increased biomass utilization as an alternative feedstock to fossil fuels. Biomass is a promising feedstock since it is abundant and cheap and can be transformed into fuels and chemical products. Microalgae biofuels are likely to have a much lower impact on the environment. Microalgae cultivation using sewage with industrial flue gases is a promising concept for integrated biodiesel production, CO₂ sequestration, and nutrients recovery. Autotrophic, Mixotrophic, and Heterotrophic are the three modes of cultivation for microalgae biomass. Several mechanical and chemical processes are available for the extraction of lipids/oily components from microalgae biomass. In organic solvent extraction methods, a prior drying of biomass and recovery of the solvent is required, which are energy-intensive. Thus, the hydrothermal process overcomes the drawbacks of conventional solvent extraction methods. In the hydrothermal process, the biomass is converted into oily components by processing in a hot, pressurized water environment. In this process, in addition to the lipid fraction of microalgae, other value-added products such as proteins, carbohydrates, and nutrients can also be recovered. In the present study was (Scenedesmus quadricauda) was isolated and cultivated in autotrophic, heterotrophic, and mixotrophically using sewage wastewater and industrial flue gas in batch and continuous mode. The harvested algae biomass from S. quadricauda was used for the recovery of lipids and bio-oil. The lipids were extracted from the algal biomass using sonication as a cell disruption method followed by solvent (Hexane) extraction, and the lipid yield obtained was 8.3 wt% with Palmitic acid, Oleic acid, and Octadeonoic acid as fatty acids. The hydrothermal process was also carried out for extraction of bio-oil, and the yield obtained was 18wt%. The bio-oil compounds such as nitrogenous compounds, organic acids, and esters, phenolics, hydrocarbons, and alkanes were obtained by the hydrothermal process of algal biomass. Nutrients such as NO₃⁻ (68%) and PO₄⁻ (15%) were also recovered along with bio-oil in the hydrothermal process.

Keywords: flue gas, hydrothermal process, microalgae, sewage wastewater, sonication

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12525 Co-Hydrothermal Gasification of Microalgae Biomass and Solid Biofuel for Biogas Production

Authors: Daniel Fozer


Limiting global warming to 1.5°C to the pre-industrial levels urges the application of efficient and sustainable carbon dioxide removal (CDR) technologies. Microalgae based biorefineries offer scalable solutions for the biofixation of CO2, where the produced biomass can be transformed into value added products by applying thermochemical processes. In this paper we report on the utilization of hydrochar as a blending component in hydrothermal gasification (HTG) process. The effects of blending ratio and hydrochar quality were investigated on the biogas yield and and composition. It is found that co-gasifying the hydrochar and the algae biomass can increase significantly the total gas yield and influence the biogas (H2, CH4, CO2, CO, C2H4, C2H6) composition. It is determined that the carbon conversion ratio, hydrogen and methane selectivity can be increased by influencing the fuel ratio of hydrochar via hydrothermal carbonization. In conclusion, it is found that increasing the synergy between hydrothermal technologies result in elevated conversion efficiency.

Keywords: biogas, CDR, Co-HTG, hydrochar, microalgae

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12524 Different Methods of Fe3O4 Nano Particles Synthesis

Authors: Arezoo Hakimi, Afshin Farahbakhsh


Herein, we comparison synthesized Fe3O4 using, hydrothermal method, Mechanochemical processes and solvent thermal method. The Hydrothermal Technique has been the most popular one, gathering interest from scientists and technologists of different disciplines, particularly in the last fifteen years. In the hydrothermal method Fe3O4 microspheres, in which many nearly monodisperse spherical particles with diameters of about 400nm, in the mechanochemical method regular morphology indicates that the particles are well crystallized and in the solvent thermal method Fe3O4 nanoparticles have good properties of uniform size and good dispersion.

Keywords: Fe3O4 nanoparticles, hydrothermal method, mechanochemical processes, solvent thermal method

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12523 Experiments on Residual Compressive Strength After Fatigue of Carbon Fiber Fabric Composites in Hydrothermal Environment

Authors: Xuan Sun, Mingbo Tong


In order to study the effect of hydrothermal environment on the fatigue properties of carbon fiber fabric composites, the experiments on fatigue and residual compressive strength with the center-hole laminates were carried out. For the experiments on fatigue in hydrothermal environment, an environmental chamber used for hydrothermal environment was designed, and the FLUENT was used to simulate the field of temperature in the environmental chamber, it proved that the design met the test requirements. In accordance with ASTM standard, the fatigue test fixture and compression test fixture were designed and produced. Then the tension-compression fatigue tests were carried out in conditions of standard environment (temperature of 23+2℃, relative humidity of 50+/-5%RH) and hydrothermal environment (temperature of 70 +2℃, relative humidity of 85+/-5%RH). After that, the residual compressive strength tests were carried out, respectively. The residual compressive strength after fatigue in condition of standard environment was set as a reference value, compared with the value in condition of hydrothermal environment, calculating the difference between them. According to the result of residual compressive strength tests, it shows that the residual compressive strength after fatigue in condition of hydrothermal environment was decreased by 13.5%,so the hydrothermal environment has little effect on the residual compressive strength of carbon fiber fabric composites laminates after fatigue under load spectrum in this research.

Keywords: carbon fiber, hydrothermal environment, fatigue, residual compressive strength

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12522 Effect of Synthesis Method on Structural, Morphological Properties of Zr0.8Y0.2-xLax Oxides (x=0, 0.1, 0.2)

Authors: Abdelaziz Ghrib, Samir Hattali, Mouloud Ghrib, Mohamed Lamine Aouissia, David Ruch


In the present study, the solid solutions with a chemical composition of Zr0.8Y0.2-xLaxO2 (x=0, 0.1, 0.2) were synthesized via two routes, by hydrothermal method using NaOH as precipitating agent at 230°C for 15h and by the sol–gel process using citric acid as complexing agent. Compounds have been characterized by powder X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Thermo gravimetric Analysis (TGA) and Differential Thermal Analysis (DTA) techniques for appropriate characterization of the distinct thermal events occurring during synthesis. All the compounds crystallize in cubic fluorite structure, as indicated by X-ray diffraction studie. The microstructure of oxides synthesized by sol-gel showed porosity that increased with the lanthanum La3+ contents compared to hydrothermal method which gives a single crystal oxide.

Keywords: oxide, hydrothermal, rare earth, solubility, sol-gel, ternary mixture

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12521 The Optimum Operating Conditions for the Synthesis of Zeolite from Waste Incineration Fly Ash by Alkali Fusion and Hydrothermal Methods

Authors: Yi-Jie Lin, Jyh-Cherng Chen


The fly ash of waste incineration processes is usually hazardous and the disposal or reuse of waste incineration fly ash is difficult. In this study, the waste incineration fly ash was converted to useful zeolites by the alkali fusion and hydrothermal synthesis method. The influence of different operating conditions (the ratio of Si/Al, the ratio of hydrolysis liquid to solid, and hydrothermal time) was investigated to seek the optimum operating conditions for the synthesis of zeolite from waste incineration fly ash. The results showed that concentrations of heavy metals in the leachate of Toxicity Characteristic Leaching Procedure (TCLP) were all lower than the regulatory limits except lead. The optimum operating conditions for the synthesis of zeolite from waste incineration fly ash by the alkali fusion and hydrothermal synthesis method were Si/Al=40, NaOH/ash=1.5, alkali fusion at 400 oC for 40 min, hydrolysis with Liquid to Solid ratio (L/S)= 200 at 105 oC for 24 h, and hydrothermal synthesis at 105 oC for 24 h. The specific surface area of fly ash could be significantly increased from 8.59 m2/g to 651.51 m2/g (synthesized zeolite). The influence of different operating conditions on the synthesis of zeolite from waste incineration fly ash followed the sequence of Si/Al ratio > hydrothermal time > hydrolysis L/S ratio. The synthesized zeolites can be reused as good adsorbents to control the air or wastewater pollutants. The purpose of fly ash detoxification, reduction and waste recycling/reuse is achieved successfully.

Keywords: alkali fusion, hydrothermal, fly ash, zeolite

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12520 Hydrothermal Liquefaction for Astaxanthin Extraction from Wet Algae

Authors: Spandana Ramisetty, Mandan Chidambaram, Ramesh Bhujade


Algal biomass is not only a potential source for biocrude but also for high value chemicals like carotenoids, fatty acids, proteins, polysaccharides, vitamins etc. Astaxanthin is one such high value vital carotenoid which has extensive applications in pharmaceutical, aquaculture, poultry and cosmetic industries and expanding as dietary supplement to humans. Green microalgae Haematococcus pluvialis is identified as the richest natural source of astaxanthin and is the key source of commercial astaxanthin. Several extraction processes from wet and dry Haematococcus pluvialis biomass have been explored by researchers. Extraction with supercritical CO₂ and various physical disruption techniques like mortar and pestle, homogenization, ultrasonication and ball mill from dried algae are widely used extraction methods. However, these processes require energy intensive drying of biomass that escalates overall costs notably. From the process economics perspective, it is vital to utilize wet processing technology in order to eliminate drying costs. Hydrothermal liquefaction (HTL) is a thermo-chemical conversion process that converts wet biomass containing over 80% water to bio-products under high temperature and high pressure conditions. Astaxanthin is a lipid soluble pigment and is usually extracted along with lipid component. Mild HTL at 200°C and 60 bar has been demonstrated by researchers in a microfluidic platform achieving near complete extraction of astaxanthin from wet biomass. There is very limited work done in this field. An integrated approach of sequential HTL offers cost-effective option to extract astaxanthin/lipid from wet algal biomass without drying algae and also recovering water, minerals and nutrients. This paper reviews past work and evaluates the astaxanthin extraction processes with focus on hydrothermal extraction.

Keywords: astaxanthin, extraction, high value chemicals, hydrothermal liquefaction

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12519 Preparation of 3D Graphene with Microwave-Hydrothermal Assistance for Ultrahigh Performance of Capacitive Deionization

Authors: Wahid Dianbudiyanto, Shou Heng Liu


Capacitive deionization (CDI) is a prospective desalination technology, which can be operated at low voltage, low temperature and potentially consume low energy for brackish water desalination. To obtain the optimal electrosorption, an electrode should possess high electrical conductivity, large surface area, good wettability, highly mesoporous structure which provide efficient pathways for ion distribution. In this work, a 3D structure graphene was fabricated using hydrothermal method which is assisted with microwave treatments to form 3D rGO (3DG-Mw-Hyd). The prepared samples have excellent specific capacitance (189.2 F / g) and ultrahigh electrosorption capacity (30 mg/g) for the desalination of 500 mg / l NaCl. These results are superior to the electrode which is fabricated only using the hydrothermal method without microwave assistance (3DG-Hyd) and traditional reflux method. Physical characterizations such as SEM, TEM, and XRD have been used to study the property difference of the materials. The preliminary results show that 3DG-Mw-Hyd is one of the promising electrodes for CDI in the practical applications.

Keywords: capacitive deionization, graphene, microwave, hydrothermal, electrosorption

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12518 Fabrication of ZnO Nanorods Based Biosensor via Hydrothermal Method

Authors: Muhammad Tariq, Jafar Khan Kasi, Samiullah, Ajab Khan Kasi


Biosensors are playing vital role in industrial, clinical, and chemical analysis applications. Among other techniques, ZnO based biosensor is an easy approach due to its exceptional chemical and electrical properties. ZnO nanorods have positively charged isoelectric point which helps immobilize the negative charge glucose oxides (GOx). Here, we report ZnO nanorods based biosensors for the immobilization of GOx. The ZnO nanorods were grown by hydrothermal method on indium tin oxide substrate (ITO). The fabrication of biosensors was carried through batch processing using conventional photolithography. The buffer solutions of GOx were prepared in phosphate with a pH value of around 7.3. The biosensors effectively immobilized the GOx and result was analyzed by calculation of voltage and current on nanostructures.

Keywords: hydrothermal growth, sol-gel, zinc dioxide, biosensors

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12517 Preparation of Protective Coating Film on Metal Alloy

Authors: Rana Th. A. Al-rubaye


A novel chromium-free protective coating films based on a zeolite coating was growing onto a FeCrAlloy metal using in –situ hydrothermal method. The zeolite film was obtained using in-situ crystallization process that is capable of coating large surfaces with complex shape and in confined spaces has been developed. The zeolite coating offers an advantage of a high mechanical stability and thermal stability. The physico-chemical properties were investigated using X-ray diffraction (XRD), Electron microscopy (SEM), Energy Dispersive X–ray analysis (EDX) and Thermogravimetric Analysis (TGA). The transition from oxide-on-alloy wires to hydrothermally synthesised uniformly zeolite coated surfaces was followed using SEM and XRD. In addition, the robustness of the prepared coating was confirmed by subjecting these to thermal cycling (ambient to 550°C).

Keywords: fecralloy, zsm-5 zeolite, zeolite coatings, hydrothermal method

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12516 Hydrothermal Aging Behavior of Continuous Carbon Fiber Reinforced Polyamide 6 Composites

Authors: Jifeng Zhang , Yongpeng Lei


Continuous carbon fiber reinforced polyamide 6 (CF/PA6) composites are potential for application in the automotive industry due to their high specific strength and stiffness. However, PA6 resin is sensitive to the moisture in the hydrothermal environment and CF/PA6 composites might undergo several physical and chemical changes, such as plasticization, swelling, and hydrolysis, which induces a reduction of mechanical properties. So far, little research has been reported on the assessment of the effects of hydrothermal aging on the mechanical properties of continuous CF/PA6 composite. This study deals with the effects of hydrothermal aging on moisture absorption and mechanical properties of polyamide 6 (PA6) and polyamide 6 reinforced with continuous carbon fibers composites (CF/PA6) by immersion in distilled water at 30 ℃, 50 ℃, 70 ℃, and 90 ℃. Degradation of mechanical performance has been monitored, depending on the water absorption content and the aging temperature. The experimental results reveal that under the same aging condition, the PA6 resin absorbs more water than the CF/PA6 composite, while the water diffusion coefficient of CF/PA6 composite is higher than that of PA6 resin because of interfacial diffusion channel. In mechanical properties degradation process, an exponential reduction in tensile strength and elastic modulus are observed in PA6 resin as aging temperature and water absorption content increases. The degradation trend of flexural properties of CF/PA6 is the same as that of tensile properties of PA6 resin. Moreover, the water content plays a decisive role in mechanical degradation compared with aging temperature. In contrast, hydrothermal environment has mild effect on the tensile properties of CF/PA6 composites. The elongation at breakage of PA6 resin and CF/PA6 reaches the highest value when their water content reaches 6% and 4%, respectively. Dynamic mechanical analysis (DMA) and scanning electron microscope (SEM) were also used to explain the mechanism of mechanical properties alteration. After exposed to the hydrothermal environment, the Tg (glass transition temperature) of samples decreases dramatically with water content increase. This reduction can be ascribed to the plasticization effect of water. For the unaged specimens, the fibers surface is coated with resin and the main fracture mode is fiber breakage, indicating that a good adhesion between fiber and matrix. However, with absorbed water content increasing, the fracture mode transforms to fiber pullout. Finally, based on Arrhenius methodology, a predictive model with relate to the temperature and water content has been presented to estimate the retention of mechanical properties for PA6 and CF/PA6.

Keywords: continuous carbon fiber reinforced polyamide 6 composite, hydrothermal aging, Arrhenius methodology, interface

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12515 The Optimization of Copper Sulfate and Tincalconite Molar Ratios on the Hydrothermal Synthesis of Copper Borates

Authors: E. Moroydor Derun, N. Tugrul, F. T. Senberber, A. S. Kipcak, S. Piskin


In this research, copper borates are synthesized by the reaction of copper sulfate pentahydrate (CuSO4.5H2O) and tincalconite (Na2O4B7.10H2O). The experimental parameters are selected as 80°C reaction temperature and 60 of reaction time. The effect of mole ratio of CuSO4.5H2O to Na2O4B7.5H2O is studied. For the identification analyses X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR) techniques are used. At the end of the experiments, synthesized copper borate is matched with the powder diffraction file of “00-001-0472” [Cu(BO2)2] and characteristic vibrations between B and O atoms are seen. The proper crystals are obtained at the mole ratio of 3:1. This study showed that simplified synthesis process is suitable for the production of copper borate minerals.

Keywords: hydrothermal synthesis, copper borates, copper sulfate, tincalconite

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12514 Catalytic Hydrothermal Decarboxylation of Lipid from Activated Sludge for Renewable Diesel Production

Authors: Ifeanyichukwu Edeh, Tim Overton, Steve Bowra


Currently biodiesel is produced from plant oils or animal’s fats by a liquid-phase catalysed transesterification process at low temperature. Although biodiesel is renewable and to a large extent sustainable, inherent properties such as poor cold flow, low oxidation stability, low cetane value restrict application to blends with fossil fuels. An alternative to biodiesel is renewable diesel produced by catalytic hydrotreating of oils and fats and is considered a drop in fuel because its properties are similar to petroleum diesel. In addition to developing alternative productions routes there is continued interest in reducing the cost of the feed stock, waste cooking oils and fats are increasingly used as the feedstocks due to low cost. However, use of oils and fat are highly adulterated resulting in high free fatty acid content which turn impacts on the efficiency of FAME production. Therefore, in light of the need to develop, alternative lipid feed stocks and related efficient catalysis the present study investigates the potential of producing renewable diesel from the lipids-extracted from activated sludge, a waste water treatment by-product, through catalytic hydrothermal decarboxylation. The microbial lipids were first extracted from the activated sludge using the Folch et al method before hydrothermal decarboxylation reactions were carried out using palladium (Pd/C) and platinum (Pt/C) on activated carbon as the catalysts in a batch reactor. The impact of three temperatures 290, 300, 330 °C and residence time between 30 min and 4hrs was assessed. At the end of the reaction, the products were recovered using organic solvents and characterized using gas chromatography (GC). The principle products of the reaction were pentadecane and heptadecane. The highest yields of pentadecane and heptadecane from lipid-extract were 23.23% and 15.21%, respectively. These yields were obtained at 290 °C and residence time 1h using Pt/C. To the best of our knowledge, the current work is the first investigation on the hydrothermal decarboxylation of lipid-extract from activated sludge.

Keywords: activated sludge, lipid, hydrothermal decarboxylation, renewable diesel

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12513 Comparative Study on Hydrothermal Carbonization as Pre- and Post-treatment of Anaerobic Digestion of Dairy Sludge: Focus on Energy Recovery, Resources Transformation and Hydrochar Utilization

Authors: Mahmood Al Ramahi, G. Keszthelyi-Szabo, S. Beszedes


Hydrothermal carbonization (HTC) is a thermochemical reaction that utilizes saturated water and vapor pressure to convert waste biomass to C-rich products This work evaluated the effect of HTC as a pre- and post-treatment technique to anaerobic digestion (AD) of dairy sludge, as information in this field is still in its infancy, with many research and methodological gaps. HTC effect was evaluated based on energy recovery, nutrients transformation, and sludge biodegradability. The first treatment approach was executed by applying hydrothermal carbonization (HTC) under a range of temperatures, prior to mesophilic anaerobic digestion (AD) of dairy sludge. Results suggested an optimal pretreatment temperature at 210 °C for 30 min. HTC pretreatment increased methane yield and chemical oxygen demand removal. The theoretical model based on Boyle’s equation had a very close match with the experimental results. On the other hand, applying HTC subsequent to AD increased total energy production, as additional energy yield was obtained by the solid fuel (hydrochar) beside the produced biogas. Furthermore, hydrothermal carbonization of AD digestate generated liquid products (HTC digestate) with improved chemical characteristics suggesting their use as liquid fertilizers.

Keywords: hydrothermal carbonization, anaerobic digestion, energy balance, sludge biodegradability, biogas

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12512 Experimental Study of Hydrothermal Properties of Cool Pavements to Mitigate Urban Heat Islands

Authors: Youssef Wardeh, Elias Kinab, Pierre Rahme, Gilles Escadeillas, Stephane Ginestet


Urban heat islands designate a local phenomenon that appears in high density cities. This results in a rise ofambient temperature in the urban area compared to the neighboring rural area. Solar radiation plays an important role in this phenomenon since it is partially absorbed by the materials, especially roads and parking lots. Cool pavements constitute an innovative and promising technique to mitigate urban heat islands. The cool pavements studied in this work allow to limit the increase of the surface temperature, thanks to evaporation of the water conducted through capillary pores, from the humidified base to the surface exposed to solar radiation. However, the performance or the cooling capacity of a pavement sometimes remained difficult to characterize. In this work, a new definition of the cooling capacity of a pavement is presented, and a correlation between the latter and the hydrothermal properties of cool pavements is revealed. Firstly, several porous concrete pavements were characterized through their hydrothermal properties, which can be related to the cooling effect, such as albedo, thermal conductivity, water absorption, etc. Secondly, these pavements initially saturated and continuously supplied with water through their bases, were exposed to external solar radiation during three sunny summer days, and their surface temperatures were measured. For draining pavements, a strong second-degreepolynomial correlation(R² = 0.945) was found between the cooling capacity and the term, which reflects the interconnection of capillary water to the surface. Moreover, it was noticed that the cooling capacity reaches its maximum for an optimal range of capillary pores for which the capillary rise is stronger than gravity. For non-draining pavements, a good negative linear correlation (R² = 0.828) was obtained between the cooling capacity and the term, which expresses the ability to heat the capillary water by the energystored far from the surface, and, therefore, the dominance of the evaporation process by diffusion. The latest tests showed that this process is, however, likely to be disturbed by the material resistance to the water vapor diffusion.

Keywords: urban heat islands, cool pavement, cooling capacity, hydrothermal properties, evaporation

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12511 Hydrothermal Synthesis of Mesoporous Carbon Nanospheres and Their Electrochemical Properties for Glucose Detection

Authors: Ali Akbar Kazemi Asl, Mansour Rahsepar


Mesoporous carbon nanospheres (MCNs) with uniform particle size distribution having an average of 290 nm and large specific surface area (274.4 m²/g) were synthesized by a one-step hydrothermal method followed by the calcination process and then utilized as an enzyme-free glucose biosensor. Morphology, crystal structure, and porous nature of the synthesized nanospheres were characterized by scanning electron microscopy (SEM), X-Ray diffraction (XRD), and Brunauer–Emmett–Teller (BET) analysis, respectively. Also, the electrochemical performance of the [email protected] electrode for the measurement of glucose concentration in alkaline media was investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and chronoamperometry (CA). [email protected] electrode shows good sensing performance, including a rapid glucose oxidation response within 3.1 s, a wide linear range of 0.026-12 mM, a sensitivity of 212.34 μA.mM⁻¹.cm⁻², and a detection limit of 25.7 μM with excellent selectivity.

Keywords: biosensor, electrochemical, glucose, mesoporous carbon, non-enzymatic

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12510 Mechanism of Formation, Mineralogy and Geochemistry of Iron Mineralization in M'Taguinarou North Tebessa, Algeria

Authors: Fakher Eddine Messaoudi


The M'Taguinarou North iron occurrence contains Iron and polymetallic mineralization (Fe-Zn-Cu), hosted in Turonian limestone. It manifests in metric clusters of goethite and hematite and in centimetre veins of smithsonite, malachite, and azurite. The genesis of this mineralization is clearly polyphased and results from the supergene processes superposed on hydrothermal phases where the Triassic diapirs probably generated the circulation of hydrothermal fluids through the sedimentary series, and the alteration of the Turonian limestone gave the formation of the hydrothermal primary ore composed of iron carbonates (siderite). Several uplift episodes affected the mineralization and the host rocks, generating the genesis of a polymetallic supergene assembly (goethite, malachite, azurite, quartz, and calcite). In M’taguinarou North, iron oxy-hydroxides are mainly observed in the form of fibrous stalactites, stalagmites, and Botroydale structures, where hematite precipitated first, followed immediately by goethite, limonite, and smithsonite. Siderite is completely absent. Subsequently, malachite, azurite, and calcite formed in the form of small veins intersecting the surrounding limestone.

Keywords: mineralization, genetic model, hydrothermal iron, supergene, Tebessa, Algeria

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12509 Reuse of Municipal Solid Waste Incinerator Fly Ash for the Synthesis of Zeolite: Effects of Different Operation Conditions

Authors: Jyh-Cherng Chen, Yi-Jie Lin


This study tries to reuse the fly ash of municipal solid waste incinerator (MSWI) for the synthesis of zeolites. The fly ashes were treated with NaOH alkali fusion at different temperatures for 40 mins and then synthesized the zeolites with hydrothermal method at 105oC for different operation times. The effects of different operation conditions and the optimum synthesis parameters were explored. The specific surface area, surface morphology, species identification, adsorption capacity, and the reuse potentials of the synthesized zeolites were analyzed and evaluated. Experimental results showed that the optimum operation conditions for the synthesis of zeolite from the mixed fly ash were Si/Al=20, alkali/ash=1.5, alkali fusion reaction with NaOH at 800oC for 40 mins, hydrolysis with L/S=200 at 105oC for 24 hr, and hydrothermal synthesis at 105oC for 48 hr. The largest specific surface area of synthesized zeolite could be increased to 943.05m2/g. The influence of different operation parameters on the synthesis of zeolite from mixed fly ash followed the sequence of Si/Al > hydrolysis L/S> hydrothermal time > alkali fusion temperature > alkali/ash ratio. The XRD patterns of synthesized zeolites were identified to be similar with the ZSM-23 zeolite. The adsorption capacities of synthesized zeolite for pollutants were increased as rising the specific surface area of synthesized zeolite. In summary, MSWI fly ash can be treated and reused to synthesize the zeolite with high specific surface area by the alkali fusion and hydrothermal method. The zeolite can be reuse for the adsorption of various pollutants. They have great potential for development.

Keywords: alkali fusion, hydrothermal, fly ash, zeolite

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12508 Lignin Valorization: Techno-Economic Analysis of Three Lignin Conversion Routes

Authors: Iris Vural Gursel, Andrea Ramirez


Effective utilization of lignin is an important mean for developing economically profitable biorefineries. Current literature suggests that large amounts of lignin will become available in second generation biorefineries. New conversion technologies will, therefore, be needed to carry lignin transformation well beyond combustion to produce energy, but towards high-value products such as chemicals and transportation fuels. In recent years, significant progress on catalysis has been made to improve transformation of lignin, and new catalytic processes are emerging. In this work, a techno-economic assessment of two of these novel conversion routes and comparison with more established lignin pyrolysis route were made. The aim is to provide insights into the potential performance and potential hotspots in order to guide the experimental research and ease the commercialization by early identifying cost drivers, strengths, and challenges. The lignin conversion routes selected for detailed assessment were: (non-catalytic) lignin pyrolysis as the benchmark, direct hydrodeoxygenation (HDO) of lignin and hydrothermal lignin depolymerisation. Products generated were mixed oxygenated aromatic monomers (MOAMON), light organics, heavy organics, and char. For the technical assessment, a basis design followed by process modelling in Aspen was done using experimental yields. A design capacity of 200 kt/year lignin feed was chosen that is equivalent to a 1 Mt/y scale lignocellulosic biorefinery. The downstream equipment was modelled to achieve the separation of the product streams defined. For determining external utility requirement, heat integration was considered and when possible gasses were combusted to cover heating demand. The models made were used in generating necessary data on material and energy flows. Next, an economic assessment was carried out by estimating operating and capital costs. Return on investment (ROI) and payback period (PBP) were used as indicators. The results of the process modelling indicate that series of separation steps are required. The downstream processing was found especially demanding in the hydrothermal upgrading process due to the presence of significant amount of unconverted lignin (34%) and water. Also, external utility requirements were found to be high. Due to the complex separations, hydrothermal upgrading process showed the highest capital cost (50 M€ more than benchmark). Whereas operating costs were found the highest for the direct HDO process (20 M€/year more than benchmark) due to the use of hydrogen. Because of high yields to valuable heavy organics (32%) and MOAMON (24%), direct HDO process showed the highest ROI (12%) and the shortest PBP (5 years). This process is found feasible with a positive net present value. However, it is very sensitive to the prices used in the calculation. The assessments at this stage are associated with large uncertainties. Nevertheless, they are useful for comparing alternatives and identifying whether a certain process should be given further consideration. Among the three processes investigated here, the direct HDO process was seen to be the most promising.

Keywords: biorefinery, economic assessment, lignin conversion, process design

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12507 Hydrothermal Synthesis of Hydrosodalite by Using Ultrasounds

Authors: B. Białecka, Z. Adamczyk, M. Cempa


The use of ultrasounds in zeolization of fly ash can increase the efficiency of this process. The molar ratios of the reagents, as well as the time and temperature of the synthesis, are the main parameters determining the type and properties of the zeolite formed. The aim of the work was to create hydrosodalite in a short time (8h), with low NaOH concentration (3 M) and in low temperature (80°C). A zeolite material contained in fly ash from hard coal combustion in one of Polish Power Plant was subjected to hydrothermal alkaline synthesis. The phase composition of the ash consisted mainly of glass, mullite, quartz, and hematite. The dominant chemical components of the ash were SiO₂ (over 50%mas.) and Al₂O₃ (more than 28%mas.), whereas the contents of the remaining components, except Fe₂O₃ (6.34%mas.), did not exceed 4% mas. The hydrothermal synthesis of the zeolite material was carried out in the following conditions: 3M-solution of NaOH, synthesis time – 8 hours, 40 kHz-frequency ultrasounds during the first two hours of synthesis. The mineral components of the input ash as well as product after synthesis were identified in microscopic observations, in transmitted light, using X-ray diffraction (XRD) and electron scanning microscopy (SEM/EDS). The chemical composition of the input ash was identified by the method of X-ray fluorescence (XRF). The obtained material apart from phases found in the initial fly ash sample, also contained new phases, i.e., hydrosodalite and NaP-type zeolite. The chemical composition in micro areas of grains indicated their diversity: i) SiO₂ content was in the range 30-59%mas., ii) Al₂O₃ content was in the range 24-35%mas., iii) Na₂O content was in the range 6-15%mas. This clearly indicates that hydrosodalite forms hypertrophies with NaP type zeolite as well as relict grains of fly ash. A small amount of potassium in the examined grains is noteworthy, which may indicate the substitution of sodium with potassium. This is confirmed by the high value of the correlation coefficient between these two components.

Keywords: fly ash, hydrosodalite, ultrasounds, zeolite

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12506 The Effect of Solution Density on the Synthesis of Magnesium Borate from Boron-Gypsum

Authors: N. Tugrul, E. Sariburun, F. T. Senberber, A. S. Kipcak, E. Moroydor Derun, S. Piskin


Boron-gypsum is a waste which occurs in the boric acid production process. In this study, the boron content of this waste is evaluated for the use in synthesis of magnesium borates and such evaluation of this kind of waste is useful more than storage or disposal. Magnesium borates, which are a sub-class of boron minerals, are useful additive materials for the industries due to their remarkable thermal and mechanical properties. Magnesium borates were obtained hydrothermally at different temperatures. Novelty of this study is the search of the solution density effects to magnesium borate synthesis process for the increasing the possibility of boron-gypsum usage as a raw material. After the synthesis process, products are subjected to XRD and FT-IR to identify and characterize their crystal structure, respectively.

Keywords: boron-gypsum, hydrothermal synthesis, magnesium borate, solution density

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12505 Effect of Synthesis Parameters on Crystal Size and Perfection of Mordenite and Analcime

Authors: Zehui Du, Chaiwat Prapainainar, Paisan Kongkachuichay, Paweena Prapainainar


The aim of this work was to obtain small crystalline size and high crystallinity of mordenites and analcimes, by modifying the aging time, agitation, water content, crystallization temperature and crystallization time. Two different hydrothermal methods were studied. Both methods used Na2SiO3 as the silica source, NaAlO2 as the aluminum source, and NaOH as the alkali source. The first method used HMI as the template while the second method did not use the template. Mordenite crystals with spherical shape and bimodal in size of about 1 and 5 µm were obtained from the first method using conditions of 24 hr aging time, 170°C and 24 hr crystallization. Modernites with high crystallinity were formed using agitation system in the crystallization process. It was also found that the aging time of 2 hr and 24 hr did not much affect the formation of mordenite crystals. Analcime crystals were formed in spherical shape and facet on surface with the size between 13-15 µm by the second method using the conditions of 30 minutes aging time, 170°C and 24 hr crystallization without calcination. By increasing water content, the crystallization process was slowed down and resulted in smaller analcime crystals. Larger size of analcime crystals were observed when the samples were calcined at 300°C and 580°C. Higher calcination temperature led to higher crystal growth and resulted in larger crystal size. Finally, mordenite and analcime was used as fillers in zeolite/Nafion composite membrane to solve the fuel cross over problem in direct alcohol fuel cell.

Keywords: analcime, hydrothermal synthesis, mordenite, zeolite

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12504 Role of Cellulose Fibers in Tuning the Microstructure and Crystallographic Phase of α-Fe₂O₃ and α-FeOOH Nanoparticles

Authors: Indu Chauhan, Bhupendra S. Butola, Paritosh Mohanty


It is very well known that properties of material changes as their size approach to nanoscale level due to the high surface area to volume ratio. However, in last few decades, a tenet ‘structure dictates function’ is quickly being adopted by researchers working with nanomaterials. The design and exploitation of nanoparticles with tailored shape and size has become one of the primary goals of materials science researchers to expose the properties of nanostructures. To date, various methods, including soft/hard template/surfactant assisted route hydrothermal reaction, seed mediated growth method, capping molecule-assisted synthesis, polyol process, etc. have been adopted to synthesize the nanostructures with controlled size and shape and monodispersity. However controlling the shape and size of nanoparticles is an ultimate challenge of modern material research. In particular, many efforts have been devoted to rational and skillful control of hierarchical and complex nanostructures. Thus in our research work, role of cellulose in manipulating the nanostructures has been discussed. Nanoparticles of α-Fe₂O₃ (diameter ca. 15 to 130 nm) were immobilized on the cellulose fiber surface by a single step in situ hydrothermal method. However, nanoflakes of α-FeOOH having thickness ca. ~25 nm and length ca. ~250 nm were obtained by the same method in absence of cellulose fibers. A possible nucleation and growth mechanism of the formation of nanostructures on cellulose fibers have been proposed. The covalent bond formation between the cellulose fibers and nanostructures has been discussed with supporting evidence from the spectroscopic and other analytical studies such as Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy. The role of cellulose in manipulating the nanostructures has been discussed.

Keywords: cellulose fibers, α-Fe₂O₃, α-FeOOH, hydrothermal, nanoflakes, nanoparticles

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12503 Hydrothermal Treatment for Production of Aqueous Co-Product and Efficient Oil Extraction from Microalgae

Authors: Manatchanok Tantiphiphatthana, Lin Peng, Rujira Jitrwung, Kunio Yoshikawa


Hydrothermal liquefaction (HTL) is a technique for obtaining clean biofuel from biomass in the presence of heat and pressure in an aqueous medium which leads to a decomposition of this biomass to the formation of various products. A role of operating conditions is essential for the bio-oil and other products’ yield and also quality of the products. The effects of these parameters were investigated in regards to the composition and yield of the products. Chlorellaceae microalgae were tested under different HTL conditions to clarify suitable conditions for extracting bio-oil together with value-added co-products. Firstly, different microalgae loading rates (5-30%) were tested and found that this parameter has not much significant to product yield. Therefore, 10% microalgae loading rate was selected as a proper economical solution for conditioned schedule at 250oC and 30 min-reaction time. Next, a range of temperature (210-290oC) was applied to verify the effects of each parameter by keeping the reaction time constant at 30 min. The results showed no linkage with the increase of the reaction temperature and some reactions occurred that lead to different product yields. Moreover, some nutrients found in the aqueous product are possible to be utilized for nutrient recovery.

Keywords: bio-oil, hydrothermal liquefaction, microalgae, aqueous co-product

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12502 The Determination of the Potassium Nitrate, Sodium Hydroxide and Boric Acid Molar Ratio in the Synthesis of Potassium Borates via Hydrothermal Method

Authors: M. Yildirim, A. S. Kipcak, F. T. Senberber, M. O. Asensio, E. M. Derun, S. Piskin


Potassium borates, which are widely used in welding and metal refining industry, as a lubricating oil additive, cement additive, fiberglass additive and insulation compound, are one of the important groups of borate minerals. In this study the production of a potassium borate mineral via hydrothermal method is aimed. The potassium source of potassium nitrate (KNO3) was used along with a sodium source of sodium hydroxide (NaOH) and boron source of boric acid (H3BO3). The constant parameters of reaction temperature and reaction time were determined as 80°C and 1 h, respectively. The molar ratios of 1:1:3 (as KNO3:NaOH:H3BO3), 1:1:4, 1:1:5, 1:1:6 and 1:1:7 were used. Following the synthesis the identifications of the produced products were conducted by X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). The results of the experiments and analysis showed in the ratio of 1:1:6, the Santite mineral with powder diffraction file number (pdf no.) of 01-072-1688, which is known as potassium pentaborate (KB5O8•4H2O) was synthesized as best.

Keywords: hydrothermal synthesis, potassium borate, potassium nitrate, santite

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12501 Synthesis of Nanoparticles and Thin Film of Cu₂ZnSnS₄ by Hydrothermal Method and Its Application as Congo Red Photocatalyst

Authors: Paula Salazar, Rodrigo Henríquez, Pablo Zerega


The textile, food and pharmaceutical industries are expanding daily worldwide, and they are located within the most polluting industries due to the fact that wastewater is discharged into watercourses with high concentrations of dyes and traces of drugs. Many of these compounds are stable to light and biodegradation, being considered as emerging organic contaminants. Advanced oxidation processes (AOPs) emerge as an effective alternative for the removal and elimination of this type of contaminants. Heterogeneous photocatalysis has been extensively studied as it is an efficient, low-cost and durable method. As the main photocatalyst, TiO₂ has been used for the degradation of a large number of dyes and drugs. The disadvantage of TiO₂ is its absorption in the UV region of the solar spectrum. On the other hand, quaternary chalcogenides based on Cu₂SnZnX₄ (X = S, Se) are a possible alternative due to their narrow bandgap (ca. between 0.8 to 1.5 eV depending on the phase considered), low cost, an abundance of its constituent elements in the earth's crust and its low toxicity. The objective of this research was to synthesize Cu₂SnZnS₄ (CZTS) through of a low-cost hydrothermal method and evaluate it as a potential photo-catalyst in the photo-degradation process of Congo Red. The synthesis of the nanoparticle in suspension and film onto fluorine-doped tin oxide coated glass (FTO) was carried out using a mixture of: 2 mmol CuCl₂, 1 mmol ZnCl₂, 1 mmol SnCl₂ and 4 mmol CH4N₂S in a Teflon reactor at 180⁰C for 72 h. Characterization was performed through scanning electron microscopy (SEM), X-ray diffraction (XRD) and UV VIS spectroscopy. Photo-degradation monitoring was carried out employing a UV VIS spectrophotometer. The results show that photodegradation of 55% of the dye can be obtained after 4h of exposure to polychromatic light, it should be noted that the Congo Red dye is being studied for the first time.

Keywords: CZTS, hydrothermal, photocatalysis, dye

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12500 Protonic Conductivity Highlighted by Impedance Measurement of Y-Doped BaZrO3 Synthesized by Supercritical Hydrothermal Process

Authors: Melanie Francois, Gilles Caboche, Frederic Demoisson, Francois Maeght, Maria Paola Carpanese, Lionel Combemale, Pascal Briois


Finding new clean, and efficient way for energy production is one of the actual global challenges. Advances in fuel cell technology have shown that, for few years, Protonic Ceramic Fuel Cell (PCFC) has attracted much attention in the field of new hydrogen energy thanks to their lower working temperature, possible higher efficiency, and better durability than classical SOFC. On the contrary of SOFC, where O²⁻ oxygen ion is the charge carrier, PCFC works with H⁺ proton as a charge carrier. Consequently, the lower activation energy of proton diffusion compared to the one of oxygen ion explains those benefits and allows PCFC to work in the 400-600°C temperature range. Doped-BaCeO₃ is currently the most chosen material for this application because of its high protonic conductivity; for example, BaCe₀.₉Y₀.₁O₃ δ exhibits a total conductivity of 1.5×10⁻²⁻¹ at 600°C in wet H₂. However, BaCeO₃ based perovskite has low stability in H₂O and/or CO₂ containing atmosphere, which limits their practical application. On the contrary, BaZrO₃ based perovskite exhibits good chemical stability but lower total conductivity than BaCeO₃ due to its larger grain boundary resistance. By substituting zirconium with 20% of yttrium, it is possible to achieve a total conductivity of 2.5×10⁻²⁻¹ at 600°C in wet H₂. However, the high refractory property of BaZr₀.₈Y₀.₂O₃-δ (noted BZY20) causes problems to obtain a dense membrane with large grains. Thereby, using a synthesis process that gives fine particles could allow better sinterability and thus decrease the number of grain boundaries leading to a higher total conductivity. In this work, BaZr₀.₈Y₀.₂O₃-δ have been synthesized by classical batch hydrothermal device and by a continuous hydrothermal device developed at ICB laboratory. The two variants of this process are able to work in supercritical conditions, leading to the formation of nanoparticles, which could be sintered at a lower temperature. The as-synthesized powder exhibits the right composition for the perovskite phase, impurities such as BaCO₃ and YO-OH were detected at very low concentration. Microstructural investigation and densification rate measurement showed that the addition of 1 wt% of ZnO as sintering aid and a sintering at 1550°C for 5 hours give high densified electrolyte material. Furthermore, it is necessary to heat the synthesized powder prior to the sintering to prevent the formation of secondary phases. It is assumed that this thermal treatment homogenizes the crystal structure of the powder and reduces the number of defects into the bulk grains. Electrochemical impedance spectroscopy investigations in various atmospheres and a large range of temperature (200-700°C) were then performed on sintered samples, and the protonic conductivity of BZY20 has been highlighted. Further experiments on half-cell, NiO-BZY20 as anode and BZY20 as electrolyte, are in progress.

Keywords: hydrothermal synthesis, impedance measurement, Y-doped BaZrO₃, proton conductor

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12499 Rare Earth Metal Ion-Doped SiO2 Nanocomposite Membranes for Gas Separation in Steam Atmosphere

Authors: Md. Hasan Zahir


Y2O3-doped silica membranes were synthesized with the sol-gel method by using a tetraethyl orthosilicate-derived sol mixed with yttrium nitrate hexahydrate. These solutions were used to fabricate hydrogen separation microporous membranes with a sandwich-type structure on γ-Al2O3 supported by tubular α-Al2O3. Pore size distribution measurements were conducted directly on the membranes before and after hydrothermal treatment with a nano-permporometer. The gas permeance properties of the membranes were measured in the temperature range 100–500°C. The Y-doped SiO2 membrane (Si/Y = 3/1) was found to exhibit asymptotically stable permeances of 2.39×10-7 mol m-2 s -1 Pa-1 for He and 6.19 ×10-10 mol m-2 s -1 Pa-1 for CO2, with a high selectivity of 386 (He/CO2) at 500°C for 20 h in the presence of steam. The Y-doped silica membranes exhibit very high gas permeances for molecules with smaller kinetic diameters. The apparent activation energies of the H2 permeance at 400°C were 24.2±0.2 and 21.3±0.7 kJ mol−1 for SiO2 and Si/Y, respectively. Very high permeances were obtained for N2 and O2, 2.2 and 5 × 10-8 mol m-2 s -1 Pa-1 respectively, which demonstrates that these materials are promising air purification and/or separation systems that block larger impurity molecules by molecular sieving effects. Y-doped SiO2 exhibits greater hydrothermal stability at high temperatures and higher selectivity than SiO2 membranes.

Keywords: ceramic membrane, gas separation, hydrothermal stability, rare earth doped-Silica

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