Search results for: temperature induced phase separation technique

Authors: Maliheh Raji, Hossein Abolghasemi, Jaber Safdari, Ali Kargari

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Dysprosium is a rare earth element which is essential for many growing high-technology applications. Dysprosium along with neodymium plays a significant role in different applications such as metal halide lamps, permanent magnets, and nuclear reactor control rods preparation. The purification and separation of rare earth elements are challenging because of their similar chemical and physical properties. Among the various methods, membrane processes provide many advantages over the conventional separation processes such as ion exchange and solvent extraction. In this work, selective extraction and separation of dysprosium from aqueous solutions containing an equimolar mixture of dysprosium and neodymium by emulsion liquid membrane (ELM) was investigated. The organic membrane phase of the ELM was a nanofluid consisting of multiwalled carbon nanotubes (MWCNT), Span80 as surfactant, Cyanex 272 as carrier, kerosene as base fluid, and nitric acid solution as internal aqueous phase. Factors affecting separation of dysprosium such as carrier concentration, MWCNT concentration, feed phase pH and stripping phase concentration were analyzed using Taguchi method. Optimal experimental condition was obtained using analysis of variance (ANOVA) after 10 min extraction. Based on the results, using MWCNT nanofluid in ELM process leads to increase the extraction due to higher stability of membrane and mass transfer enhancement and separation factor of 6 for dysprosium over neodymium can be achieved under the optimum conditions. Additionally, demulsification process was successfully performed and the membrane phase reused effectively in the optimum condition.

Keywords: emulsion liquid membrane, MWCNT nanofluid, separation, Taguchi method

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Authors: Arseniy M. Kondratyev, Sergey V. Onufriev, Alexander I. Savvatimskiy

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The microsecond electrical pulse heating technique which provides uniform energy input into an investigated specimen is considered. In the present study we investigated ZrC+C carbide specimens in a form of a thin layer (about 5 microns thick) that were produced using a method of magnetron sputtering on insulating substrates. Specimens contained (at. %): Zr–17.88; C–67.69; N–8.13; O–5.98. Current through the specimen, voltage drop across it and radiation at the wavelength of 856 nm were recorded in the experiments. It enabled us to calculate the input energy, specific heat (from 2300 to 4500 K) and resistivity (referred to the initial dimensions of a specimen). To obtain the true temperature a black body specimen was used. Temperature of the beginning and completion of a phase transition (solid–liquid) was measured.Temperature of the onset of melting was 3150 K at the input energy 2.65 kJ/g; temperature of the completion of melting was 3450 K at the input energy 5.2 kJ/g. The specific heat of the solid phase of investigated carbide calculated using our data on temperature and imparted energy, is close to 0.75 J/gК for temperature range 2100–2800 K. Our results are considered together with the equilibrium Zr-C phase diagram.

Keywords: pulse heating, zirconium carbide, high temperatures, melting

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Authors: Quy Dang Nguyen, Reza Nakhaie Jazar

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The paper investigates vibration dynamics of tire-road separation for a quarter-car model; this separation model is developed to be close to the real situation considering the tire is able to separate from the ground plane. A set of piecewise linear mathematical models is developed and matches the in-contact and no-contact states to be considered as mother models for further investigations. The bound dynamics are numerically simulated in the time response and phase portraits. The separation analysis may determine which values of suspension parameters can delay and avoid the no-contact phenomenon, which results in improving ride comfort and eliminating the potentially dangerous oscillation. Finally, model verification is carried out in the MSC-ADAMS environment.

Keywords: quarter-car vibrations, tire-road separation, separation analysis, separation dynamics, ride comfort, ADAMS validation

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Authors: Ravi V. Joat, Pravin S. Bodke, Shradha S. Binani, S. S. Wasnik

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A phase diagram of the Ag2SO4 - CaSO4 (Silver sulphate – Calcium Sulphate) binaries system using conductivity, XRD (X-Ray Diffraction Technique) and DTA (Differential Thermal Analysis) data is constructed. The eutectic reaction (liquid -» a-Ag2SO4 + CaSO4) is observed at 10 mole% CaSO4 and 645°C. Room temperature solid solubility limit up to 5.27 mole % of Ca 2+ in Ag2SO4 is set using X-ray powder diffraction and scanning electron microscopy results. All compositions beyond this limit are two-phase mixtures below and above the transition temperature (≈ 416°C). The bulk conductivity, obtained following complex impedance spectroscopy, is found decreasing with increase in CaSO4 content. Amongst other binary compositions, the 80AgSO4-20CaSO4 gave improved sinterability/packing density.

Keywords: phase diagram, Ag2SO4-CaSO4 binaries system, conductivity, XRD, DTA

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Authors: Rana Muhammad Armaghan Ayaz, Yigit Uysallı, Nima Bavili, Berna Morova, Alper Kiraz

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Traditional optical methods for example resonance wavelength shift and cavity ring-down spectroscopy used for material detection and sensing have disadvantages, for example, less resistance to laser noise, temperature fluctuations and extraction of the required information can be a difficult task like ring downtime in case of cavity ring-down spectroscopy. Phase shift cavity ring down spectroscopy is not only easy to use but is also capable of overcoming the said problems. This technique compares the phase difference between the signal coming out of the cavity with the reference signal. Detection of any material is made by the phase difference between them. By using this technique, air, water, and isopropyl alcohol can be recognized easily. This Methodology has far-reaching applications and can be used in air pollution detection, human breath analysis and many more.

Keywords: materials, noise, phase shift, resonance wavelength, sensitivity, time domain approach

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Authors: Wiqar Hussain Shah

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The Structural, magnetic and transport behavior of La1-xCaxMnO3+ (x=0.48, 0.50, 0.52 and 0.55 and =0.015) compositions close to charge ordering, was studied through XRD, resistivity, DC magnetization and AC susceptibility measurements. With time and thermal cycling (T<300 K) there is an irreversible transformation of the low-temperature phase from a partially ferromagnetic and metallic to one that is less ferromagnetic and highly resistive. For instance, an increase of resistivity can be observed by thermal cycling, where no effect is obtained for lower Ca concentration. The time changes in the magnetization are logarithmic in general and activation energies are consistent with those expected for electron transfer between Mn ions. The data suggest that oxygen non-stoichiometry results in mechanical strains in this two-phase system, leading to the development of irreversible metastable states, which relax towards the more stable charge-ordered and antiferromagnetic microdomains at the nano-meter size. This behavior is interpreted in terms of strains induced charge localization at the interface between FM/AFM domains in the antiferromagnetic matrix. Charge, orbital ordering and phase separation play a prominent role in the appearance of such properties, since they can be modified in a spectacular manner by external factor, making the different physical properties metastable. Here we describe two factors that deeply modify those properties, viz. the doping concentration and the thermal cycling. The metastable state is recovered by the high temperature annealing. We also measure the magnetic relaxation in the metastable state and also the revival of the metastable state (in a relaxed sample) due to high temperature (800 ) thermal treatment.

Keywords: Rare-earth maganites, nano-structural materials, doping effects on electrical, magnetic properties, competing interactions

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Authors: Baobao Chang, Konrad Schneider, Vogel Roland, Gert Heinrich

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In this work, the influence of annealing on the mechanical αc-relaxation behavior of isotactic polypropylene (iPP) was investigated. The results suggest that the mechanical αc-relaxation behavior depends strongly on the confinement force on the polymer chains in the intermediate phase and the thickness of the intermediate phase. After quenching at 10°C, abundant crystallites with a wide size distribution are formed. The polymer chains in the intermediate phase are constrained by the crystallites, giving rise to one broad αc-relaxation peak. With an annealing temperature between 60°C~105°C, imperfect lamellae melting releases part of the constraint force, which reduces the conformational ordering of the polymer chains neighboring the amorphous phase. Consequently, two separate αc-relaxation peaks could be observed which are labeled as αc1-relaxation and αc2-relaxation. αc1-relaxation and αc2-relaxation describe the relaxation behavior of polymer chains in the region close to the amorphous phase and the crystalline phase, respectively. Both relaxation peaks shift to a higher temperature as annealing temperature increases. With an annealing temperature higher than 105°C, the new crystalline phase is formed in the intermediate phase, which enhances the constraint force on the polymer chains. αc1-relaxation peak is broadened obviously and its position shifts to a higher temperature as annealing temperature increases. Moreover, αc2-relaxation is undetectable because that the polymer chains in the region between the initial crystalline phase and the newly formed crystalline phase are strongly confined.

Keywords: annealing, αc-relaxation, isotactic-polypropylene, intermediate phase

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Authors: Hiroshi Katanoda, Mohd Hazwan bin Yusof

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A theoretical investigation from the viewpoint of gas-dynamics and thermodynamics was carried out, in order to clarify the energy separation mechanism in a viscous compressible vortex, as a primary flow element in a uni-flow vortex tube. The mathematical solutions of tangential velocity, density and temperature in a viscous compressible vortical flow were used in this study. It is clear that a total temperature in the vortex core falls well below that distant from the vortex core in the radial direction, causing a region with higher total temperature, compared to the distant region, peripheral to the vortex core.

Keywords: energy separation mechanism, theoretical analysis, vortex tube, vortical flow

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Authors: Ozan Kahraman, Hao Feng

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Ultrasonic atomization (UA) is a useful technique for producing a liquid spray for various processes, such as spray drying. Ultrasound generates small droplets (a few microns in diameter) by disintegration of the liquid via cavitation and/or capillary waves, with low range velocity and narrow droplet size distribution. In recent years, UA has been investigated as an alternative for enabling or enhancing ultrasound-mediated unit operations, such as evaporation, separation, and purification. The previous studies on the UA separation of a solvent from a bulk solution were limited to ethanol-water systems. More investigations into ultrasound-mediated separation for other liquid systems are needed to elucidate the separation mechanism. This study was undertaken to investigate the effects of the operational parameters on the ultrasound-mediated separation of three miscible liquid pairs: ethanol-, methanol-, and butanol-water. A 2.4 MHz ultrasonic mister with a diameter of 18 mm and rating power of 24 W was installed on the bottom of a custom-designed cylindrical separation unit. Air was supplied to the unit (3 to 4 L/min.) as a carrier gas to collect the mist. The effects of the initial alcohol concentration, viscosity, and temperature (10, 30 and 50°C) on the atomization rates were evaluated. The alcohol concentration in the collected mist was measured with high performance liquid chromatography and a refractometer. The viscosity of the solutions was determined using a Brookfield digital viscometer. The alcohol concentration of the atomized mist was dependent on the feed concentration, feed rate, viscosity, and temperature. Increasing the temperature of the alcohol-water mixtures from 10 to 50°C increased the vapor pressure of both the alcohols and water, resulting in an increase in the atomization rates but a decrease in the separation efficiency. The alcohol concentration in the mist was higher than that of the alcohol-water equilibrium at all three temperatures. More importantly, for ethanol, the ethanol concentration in the mist went beyond the azeotropic point, which cannot be achieved by conventional distillation. Ultrasound-mediated separation is a promising non-equilibrium method for separating and purifying alcohols, which may result in significant energy reductions and process intensification.

Keywords: azeotropic mixtures, distillation, evaporation, purification, seperation, ultrasonic atomization

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Authors: Devi Eka Septiyani Arifin, Jrjeng Ruan

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As an approach to manipulate the performance of polymer thin film, epitaxy crystallization within polymer blends of poly(vinylidene fluoride) (PVDF) and its copolymer poly(vinylidene fluoride-trifluoroethylene) P(VDF-TrFE) was studied in this research, which involves the competition between phase separation and crystal growth of constitutive semicrystalline polymers. The unique piezoelectric feature of poly(vinylidene fluoride) crystalline phase is derived from the packing of molecular chains in all-trans conformation, which spatially arranges all the substituted fluorene atoms on one side of the molecular chain and hydrogen atoms on the other side. Therefore, the net dipole moment is induced across the lateral packing of molecular chains. Nevertheless, due to the mutual repulsion among fluorene atoms, this all-trans molecular conformation is not stable, and ready to change above curie temperature, where thermal energy is sufficient to cause segmental rotation. This research attempts to explore whether the epitaxial interactions between piezoelectric crystals and crystal lattice of hexamethylbenzene (HMB) crystalline platelet is able to stabilize this metastable all-trans molecular conformation or not. As an aromatic crystalline compound, the melt of HMB was surprisingly found able to dissolve the poly(vinylidene fluoride), resulting in homogeneous eutectic solution. Thus, after quenching this binary eutectic mixture to room temperature, subsequent heating or annealing processes were designed to explore the involve phase separation and crystallization behavior. The phase transition behaviors were observed in-situ by X-ray diffraction and differential scanning calorimetry (DSC). The molecular packing was observed via transmission electron microscope (TEM) and the principles of electron diffraction were brought to study the internal crystal structure epitaxially developed within thin films. Obtained results clearly indicated the occurrence of heteroepitaxy of PVDF/PVDF-TrFE on HMB crystalline platelet. Both the concentration of poly(vinylidene fluoride) and the mixing ratios of these two constitutive polymers have been adopted as the influential factors for studying the competition between the epitaxial crystallization of PVDF and P(VDF-TrFE) on HMB crystalline. Furthermore, the involved epitaxial relationship is to be deciphered and studied as a potential factor capable of guiding the wide spread of piezoelectric crystalline form.

Keywords: epitaxy, crystallization, crystalline platelet, thin film and mixing ratio

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Authors: Woei-Shyan Lee, Yu-Liang Chuang

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The nano-mechanical properties of as-deposited Cu/Si thin films indented to a depth of 2000 nm are investigated using a nanoindentation technique. The nanoindented specimens are annealed at a temperature of either 160 °C or 210°C, respectively. The microstructures of the as-deposited and annealed samples are then examined via transmission electron microscopy (TEM). The results show that both the loading and the unloading regions of the load-displacement curve are smooth and continuous, which suggests that no debonding or cracking occurs during nanoindentation. In addition, the hardness and Young’s modulus of the Cu/Si thin films are found to vary with the nanoindentation depth, and have maximum values of 2.8 GPa and 143 GPa, respectively, at the maximum indentation depth of 2000 nm. The TEM observations show that the region of the Cu/Si film beneath the indenter undergoes a phase transformation during the indentation process. In the case of the as-deposited specimens, the indentation pressure induces a completely amorphous phase within the indentation zone. For the specimens annealed at a temperature of 160°C, the amorphous nature of the microstructure within the indented zone is maintained. However, for the specimens annealed at a higher temperature of 210°C, the indentation affected zone consists of a mixture of amorphous phase and nanocrystalline phase. Copper silicide (η-Cu3Si) precipitates are observed in all of the annealed specimens. The density of the η-Cu3Si precipitates is found to increase with an increasing annealing temperature.

Keywords: nanoindentation, Cu/Si thin films, microstructural evolution, annealing temperature

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Authors: Perumalsamy Muthiah, Murugesan Thanapalan

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The remains of cheese production contain nutritional value added proteins viz., α-Lactalbumin, β-Lactoglobulin representing 80- 90% of the total volume of milk entering the process. Although several possibilities for cheese-whey exploitation have been assayed, approximately half of world cheese-whey production is not treated but is discarded as effluent. It is necessary to develop an effective and environmentally benign extraction process for the recovery of value added cheese whey proteins. Recently aqueous two phase system (ATPS) have emerged as potential separation process, particularly in the field of biotechnology due to the mild conditions of the process, short processing time, and ease of scale-up. In order to design an ATPS process for the recovery of cheese whey proteins, development of phase diagram and the effect of system parameters such as pH, types and the concentrations of the phase forming components, temperature, etc., on the partitioning of proteins were addressed in order to maximize the recovery of proteins. Some of the practical problems encountered in the application of aqueous two-phase systems for the recovery of Cheese whey proteins were also discussed.

Keywords: aqueous two-phase system, phase diagram, extraction, cheese whey

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Authors: M. Akif Ceviz, Alirıza Kaleli, Erdoğan Güner

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LPG pressure regulator is a device which is used to change the phase of LPG from liquid to gas by decreasing the pressure. During the phase change, it is necessary to supply the latent heat of LPG to prevent excessive low temperature. Engine coolant is circulated in the pressure regulator for this purpose. Therefore, pressure regulator is a type of heat exchanger that should be designed for different engine operating conditions. The design of the regulator should ensure that the flow of LPG is in gaseous phase to the injectors during the engine steady state and transient operating conditions. The pressure regulators in the LPG gaseous injection systems currently used can easily change the phase of LPG, however, there is no any control on the LPG temperature in conventional LPG injection systems. It is possible to increase temperature excessively. In this study, a control unit has been tested to keep the LPG temperature in a band. Result of the study showed that the engine performance characteristics can be increased by using the system.

Keywords: temperature, pressure regulator, LPG, PID

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Authors: Hui Zhu, Yuan Wang, Shibo Kuang, Aibing Yu

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The inertial difference induced by the microfluidics inside a curved micro-channel has great potential to provide a fast, inexpensive, and portable solution to the separation of micro- and sub-micro particles in many applications such as aerosol collections, airborne bacteria and virus detections, as well as particle sortation. In this work, the separation behaviors of different sized particles inside a reported curved micro-channel have been studied by a combined approach of computational fluid dynamics for gas and discrete element model for particles (CFD-DEM). The micro-channel is operated by controlling the gas flow rates at all of its branches respectively used to load particles, introduce gas streams, collect particles of various sizes. The validity of the model has been examined by comparing by the calculated separation efficiency of different sized particles against the measurement. On this basis, the separation mechanisms of the inertial microfluidic separator are elucidated in terms of the interactions between particles, between particle and fluid, and between particle and wall. The model is then used to study the effect of feed solids concentration on the separation accuracy and efficiency. The results obtained from the present study demonstrate that the CFD-DEM approach can provide a convenient way to study the particle separation behaviors in micro-channels of various types.

Keywords: CFD-DEM, inertial effect, microchannel, separation

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Authors: Woei-Shyan Lee, Shuo-Ling Chang

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The nanoindentation behaviour and phase transformation of annealed single-crystal silicon wafers are examined. The silicon specimens are annealed at temperatures of 250, 350 and 450ºC, respectively, for 15 minutes and are then indented to maximum loads of 30, 50 and 70 mN. The phase changes induced in the indented specimens are observed using transmission electron microscopy (TEM) and micro-Raman scattering spectroscopy (RSS). For all annealing temperatures, an elbow feature is observed in the unloading curve following indentation to a maximum load of 30 mN. Under higher loads of 50 mN and 70 mN, respectively, the elbow feature is replaced by a pop-out event. The elbow feature reveals a complete amorphous phase transformation within the indented zone, whereas the pop-out event indicates the formation of Si XII and Si III phases. The experimental results show that the formation of these crystalline silicon phases increases with an increasing annealing temperature and indentation load. The hardness and Young’s modulus both decrease as the annealing temperature and indentation load are increased.

Keywords: nanoindentation, silicon, phase transformation, amorphous, annealing

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Authors: Kul Pun, F. A. Hamad, T. Ahmed, J. O. Ugwu, J. Eyers, G. Lawson, P. A. Russell

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Determining droplet size and distribution is essential when determining the separation efficiency of a two/three-phase separator. This paper investigates the effect of liquid flow and oil pad thickness on the droplet size at the lab scale. The findings show that increasing the inlet flow rates of the oil and water results in size reduction of the droplets and increasing the thickness of the oil pad increases the size of the droplets. The data were fitted with a simple Gaussian model, and the parameters of mean, standard deviation, and amplitude were determined. Trends have been obtained for the fitted parameters as a function of the Reynolds number, which suggest a way forward to better predict the starting parameters for population models when simulating separation using CFD packages. The key parameter to predict to fix the position of the Gaussian distribution was found to be the mean droplet size.

Keywords: two-phase separator, average bubble droplet, bubble size distribution, liquid-liquid phase

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Authors: N. Zanganeh, M. Zabet

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Lactulose is a synthetic disaccharide which has remarkable applications in food and pharmaceutical fields. Lactulose is not found in nature and it is produced by isomerization reaction of lactose in an alkaline environment. It should be noted that this reaction has a very low yield since significant amount of lactose stays un-reacted in the system. Basically, purification of lactulose is difficult and costly. Previous studies have revealed that solubility of lactose and lactulose are significantly different in ethanol. Considering the fact that solubility is also affected by temperature itself, we investigated the effect of ethanol and temperature on separation process of lactose from the syrup containing lactose and lactulose. For this purpose, a saturated solution containing lactulose and lactose was made at three different temperatures; 25⁰C (room temperature), 31⁰C, and 37⁰C first.  Five samples containing 2g saturated solution was taken and then 2g, 3g, 4g, 5g, and 6g ethanol separately was added to the sampling tubes. Sampling tubes were kept at respective temperatures afterward. The concentration of lactose and lactulose after separation process measured and analyzed by High Performance Liquid Chromatography (HPLC). Results showed that ethanol has such a greater impact than operating temperature on purification process. Also, it was observed that the maximum rate of separation occurred at initial amount of added ethanol.

Keywords: lactulose, lactose, purification, solubility

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Authors: Adesoji Sodeinde

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Analytical derivatives has recently undergone an explosive growth in areas of separation techniques, likewise in detectability of certain compound/concentrated ions. The gloomy and depressing scenario which charaterized the application of analytical derivatives in areas of water analysis, water cycle and the environment should not be allowed to continue unabated. Due to technological advancement in various chemical/biochemical analysis separation techniques is widely used in areas of medical, forensic and to measure and assesses environment and social-economic impact of alternative control strategies. This technological improvement was dully established in the area of comparison between certain separation/detection techniques to bring about vital result in forensic[as Gas liquid chromatography reveals the evidence given in court of law during prosecution of drunk drivers]. The water quality analysis,pH and water temperature analysis can be performed in the field, the concentration of dissolved free amino-acid [DFAA] can also be detected through separation techniques. Some important derivatives/ions used in separation technique. Water analysis : Total water hardness [EDTA to determine ca and mg ions]. Gas liquid chromatography : innovative gas such as helium [He] or nitrogen [N] Water cycle : Animal bone charcoal,activated carbon and ultraviolet light [U.V light].

Keywords: analytical derivative, environment, water analysis, chemical/biochemical analysis

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Authors: Homoud Bourisli, Haitham Safar

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Oil is one of main resources of energy in the world. As conventional oil is drying out, oil recovery is crucial to maintain the same level of oil production. Since water injection is one of the commonly used methods to increase and maintain pressure in oil wells, oil-water separation processes of the water associated with oil production for water injection oil recovery is very essential. Therefore, Gas Flotation Units are used for oil-water separation to be able to re-inject the treated water back into the wells to increase pressure.

Keywords: Kuwait oil company, dissolved gas flotation unit, induced gas flotation unit, oil-water separation

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Authors: Haiming Wen

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Grain growth is an important and consequential phenomenon that generally occurs in the presence of thermal and/or stress/strain fields. Thermally activated grain growth has been extensively studied and similarly, there are numerous experimental and theoretical studies published describing stress-induced grain growth in single-phase materials. However, studies on grain growth during the simultaneous presence of an elevated temperature and an external stress are very limited, and moreover, grain growth phenomena in materials containing second-phase particles and solute segregation at GBs have received limited attention. This lecture reports on a study of grain growth in the presence of second-phase particles and solute/impurity segregation at grain boundaries (GBs) during high-temperature deformation of an ultra-fine grained (UFG) Al alloy synthesized via consolidation of mechanically milled powders. The mechanisms underlying the grain growth were identified as GB migration and grain rotation, which were accompanied by dynamic recovery and geometric dynamic recrystallization, while discontinuous dynamic recrystallization was not operative. A theoretical framework that incorporates the influence of second-phase particles and solute/impurity segregation at GBs on grain growth in presence of both elevated temperature and external stress is formulated and discussed. The effect of second-phase particles and solute/impurity segregation at GBs on GB migration and grain rotation was quantified using the proposed theoretical framework, indicating that both second-phase particles and solutes/impurities segregated GBs reduce the velocities of GB migration and grain rotation as compared to those in commercially pure Al. Our results suggest that grain growth predicted by the proposed theoretical framework is in agreement with experimental results. Hence, the developed theoretical framework can be applied to quantify grain growth in simultaneous presence of external stress, elevated temperature, GB segregation and second-phase particles, or in presence of one or more of the aforementioned factors.

Keywords: nanocrystalline materials, ultra-fine grained materials, grain growth, grain boundary migration, grain rotation

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Authors: Nikola Toshikj, Michel Ramonda, Sylvain Catrouillet, Jean-Jacques Robin, Sebastien Blanquer

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Biodegradable and biocompatible block copolymers have risen as the golden materials in both medical and environmental applications. Moreover, if their architecture is of controlled manner, higher applications can be foreseen. In the meantime, organocatalytic ROP has been promoted as more rapid and immaculate route, compared to the traditional organometallic catalysis, towards efficient synthesis of block copolymer architectures. Therefore, herein we report novel organocatalytic pathway with guanidine molecules (TBD) for supported synthesis of trimethylene carbonate initiated by poly(caprolactone) as pre-polymer. Pristine PTMC-b-PCL-b-PTMC block copolymer structure, without any residual products and clear desired block proportions, was achieved under 1.5 hours at room temperature and verified by NMR spectroscopies and size-exclusion chromatography. Besides, when elaborating block copolymer films, further stability and amelioration of mechanical properties can be achieved via additional reticulation step of precedently methacrylated block copolymers. Subsequently, stimulated by the insufficient studies on the phase-separation/crystallinity relationship in these semi-crystalline block copolymer systems, their intrinsic thermal and morphology properties were investigated by differential scanning calorimetry and atomic force microscopy. Firstly, by DSC measurements, the block copolymers with χABN values superior to 20 presented two distinct glass transition temperatures, close to the ones of the respecting homopolymers, demonstrating an initial indication of a phase-separated system. In the interim, the existence of the crystalline phase was supported by the presence of melting temperature. As expected, the crystallinity driven phase-separated morphology predominated in the AFM analysis of the block copolymers. Neither crosslinking at melted state, hence creation of a dense polymer network, disturbed the crystallinity phenomena. However, the later revealed as sensible to rapid liquid nitrogen quenching directly from the melted state. Therefore, AFM analysis of liquid nitrogen quenched and crosslinked block copolymer films demonstrated a thermodynamically driven phase-separation clearly predominating over the originally crystalline one. These AFM films remained stable with their morphology unchanged even after 4 months at room temperature. However, as demonstrated by DSC analysis once rising the temperature above the melting temperature of the PCL block, neither the crosslinking nor the liquid nitrogen quenching shattered the semi-crystalline network, while the access to thermodynamical phase-separated structures was possible for temperatures under the poly (caprolactone) melting point. Precisely this coexistence of dual crosslinked/crystalline networks in the same copolymer structure allowed us to establish, for the first time, the shape-memory properties in such materials, as verified by thermomechanical analysis. Moreover, the response temperature to the material original shape depended on the block copolymer emplacement, hence PTMC or PCL as end-block. Therefore, it has been possible to reach a block copolymer with transition temperature around 40°C thus opening potential real-life medical applications. In conclusion, the initial study of phase-separation/crystallinity relationship in PTMC-b-PCL-b-PTMC block copolymers lead to the discovery of novel shape memory materials with superior properties, widely demanded in modern-life applications.

Keywords: biodegradable block copolymers, organocatalytic ROP, self-assembly, shape-memory

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Authors: A. Bouloufa, K. Djessas

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In this paper, we reported the effect of substrate temperature on the structural, electrical and optical properties of In2S3 thin films deposited on soda-lime glass substrates by physical vapor deposition technique at various substrate temperatures. The In2Se3 material used for deposition was synthesized from its constituent elements. It was found that all samples exhibit one phase which corresponds to β-In2S3 phase. Values of band gap energy of the films obtained at different substrate temperatures vary in the range of 2.38-2.80 eV and decrease with increasing substrate temperature.

Keywords: buffer layer, In2S3, optical properties, PVD, structural properties

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Authors: Alexandra C. Blaga, Dan Caşcaval, Alexandra Tucaliuc, Madalina Poştaru, Anca I. Galaction

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Amino acids are valuable chemical products used in in human foods, in animal feed additives and in the pharmaceutical field. Recently, there has been a noticeable rise of amino acids utilization throughout the world to include their use as raw materials in the production of various industrial chemicals: oil gelating agents (amino acid-based surfactants) to recover effluent oil in seas and rivers and poly(amino acids), which are attracting attention for biodegradable plastics manufacture. The amino acids can be obtained by biosynthesis or from protein hydrolysis, but their separation from the obtained mixtures can be challenging. In the last decades there has been a continuous interest in developing processes that will improve the selectivity and yield of downstream processing steps. The liquid-liquid extraction of amino acids (dissociated at any pH-value of the aqueous solutions) is possible only by using the reactive extraction technique, mainly with extractants of organophosphoric acid derivatives, high molecular weight amines and crown-ethers. The purpose of this study was to analyse the separation of nine amino acids of acidic character (l-aspartic acid, l-glutamic acid), basic character (l-histidine, l-lysine, l-arginine) and neutral character (l-glycine, l-tryptophan, l-cysteine, l-alanine) by reactive extraction with di-(2-ethylhexyl)phosphoric acid (D2EHPA) dissolved in butyl acetate. The results showed that the separation yield is controlled by the pH value of the aqueous phase: the reactive extraction of amino acids with D2EHPA is possible only if the amino acids exist in aqueous solution in their cationic forms (pH of aqueous phase below the isoeletric point). The studies for individual amino acids indicated the possibility of selectively separate different groups of amino acids with similar acidic properties as a function of aqueous solution pH-value: the maximum yields are reached for a pH domain of 2–3, then strongly decreasing with the pH increase. Thus, for acidic and neutral amino acids, the extraction becomes impossible at the isolelectric point (pHi) and for basic amino acids at a pH value lower than pHi, as a result of the carboxylic group dissociation. From the results obtained for the separation from the mixture of the nine amino acids, at different pH, it can be observed that all amino acids are extracted with different yields, for a pH domain of 1.5–3. Over this interval, the extract contains only the amino acids with neutral and basic character. For pH 5–6, only the neutral amino acids are extracted and for pH > 6 the extraction becomes impossible. Using this technique, the total separation of the following amino acids groups has been performed: neutral amino acids at pH 5–5.5, basic amino acids and l-cysteine at pH 4–4.5, l-histidine at pH 3–3.5 and acidic amino acids at pH 2–2.5.

Keywords: amino acids, di-(2-ethylhexyl) phosphoric acid, reactive extraction, selective extraction

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Authors: Zhipeng Feng, Huanhuan Qi, Pingchuan Shen, Fenggang Zang, Yixiong Zhang

Abstract:

Numerical simulations of vortex-induced vibration of a three-dimensional flexible tube under uniform turbulent flow are calculated when Reynolds number is 1.35×10⁴. In order to achieve the vortex-induced vibration, the three-dimensional unsteady, viscous, incompressible Navier-Stokes equation and LES turbulence model are solved with the finite volume approach, the tube is discretized according to the finite element theory, and its dynamic equilibrium equations are solved by the Newmark method. The fluid-tube interaction is realized by utilizing the diffusion-based smooth dynamic mesh method. Considering the vortex-induced vibration system, the variety trends of lift coefficient, drag coefficient, displacement, vertex shedding frequency, phase difference angle of tube are analyzed under different frequency ratios. The nonlinear phenomena of locked-in, phase-switch are captured successfully. Meanwhile, the limit cycle and bifurcation of lift coefficient and displacement are analyzed by using trajectory, phase portrait, and Poincaré sections. The results reveal that: when drag coefficient reaches its minimum value, the transverse amplitude reaches its maximum, and the “lock-in” begins simultaneously. In the range of lock-in, amplitude decreases gradually with increasing of frequency ratio. When lift coefficient reaches its minimum value, the phase difference undergoes a suddenly change from the “out-of-phase” to the “in-phase” mode.

Keywords: vortex induced vibration, limit cycle, LES, CFD, FEM

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Authors: Ramin Dabirian, Yi Zhang, Ilias Gavrielatos, Ram Mohan, Ovadia Shoham

Abstract:

Oil-water emulsions can be found in almost every part of the petroleum industry, namely in reservoir rocks, drilling cuttings circulation, production in wells, transportation pipelines, surface facilities and refining process. However, it is necessary for oil production and refinery engineers to resolve the petroleum emulsion problems as well as to eliminate the contaminants in order to meet environmental standards, achieve the desired product quality and to improve equipment reliability and efficiency. A state-of-art Dispersion Characterization Rig (DCR) has been utilized to investigate crude oil-distilled water dispersion separation. Over 80 experimental tests were ran to investigate the flow behavior and stability of the dispersions. The experimental conditions include the effects of water cuts (25%, 50% and 75%), NaCl concentrations (0, 3.5% and 18%), mixture flow velocities (0.89 and 1.71 ft/s), and also orifice place types on the separation rate. The experimental data demonstrate that the water cut can significantly affects the separation time and efficiency. The dispersion with lower water cut takes longer time to separate and have low separation efficiency. The medium and lower water cuts will result in the formation of Mousse emulsion and the phase inversion happens around the medium water cut. The data also confirm that increasing the NaCl concentration in aqueous phase can increase the crude oil water dispersion separation efficiency especially at higher salinities. The separation profile for dispersions with lower salt concentrations has a lower sedimentation rate slope before the inflection point. Dispersions in all tests with higher salt concentrations have a larger sedimenting rate. The presence of NaCl can influence the interfacial tension gradients along the interface and it plays a role in avoiding the Mousse emulsion formation.

Keywords: oil-water dispersion, separation mechanism, phase inversion, emulsion formation

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Authors: Salim Al Jadidi, Shian Gao, Shivananda Moolya

Abstract:

Computational Fluid Dynamic (CFD) technique coupled with Sub-Grid-Scale (SGS) model is used to study the flow behavior of heavy oil-water-air flow in a horizontal pipe by adapting ANSYS Fluent CFD software. The technique suitable for the transport of water-lubricated heavy viscous oil in a horizontal pipe is the Core Annular flow (CAF) technique. The present study focuses on the numerical study of CAF adapting Large Eddy Simulations (LES). The basic objective of the present study is to gain a basic knowledge of the flow behavior of heavy oil using turbulent CAF through a conventional horizontal pipe. This work also focuses on the success and applicability of LES. The simulation of heavy oil-water-air three-phase flow and two-phase flow of heavy oil–water in a conventional horizontal pipe is performed using ANSYS Fluent 16.2 software. The influence of three-phase heavy oil-water air flow in a selected pipe is affected by gravity. It is also observed from the result that the air phase and the variation in the temperature impact the behavior of the annular stream and pressure drop. Some results obtained during the study are validated with the results gained from part of the literature experiments and simulations, and the results show reasonably good agreement between the studies.

Keywords: computational fluid dynamics, gravity, heavy viscous oil, three-phase flow

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Authors: Wei-Song Hung

Abstract:

We utilized pressure, vacuum, and evaporation-assisted self-assembly techniques through which graphene oxide (GO) was deposited on modified polyacrylonitrile (mPAN). The fabricated composite GO/mPAN membranes were applied to dehydrate 1-butanol mixtures by pervaporation. Varying driving forces in the self-assembly techniques induced different GO assembly layer microstructures. XRD results indicated that the GO layer d-spacing varied from 8.3 Å to 11.5 Å. The self-assembly technique with evaporation resulted in a heterogeneous GO layer with loop structures; this layer was shown to be hydrophobic, in contrast to the hydrophilic layer formed from the other two techniques. From the pressure-assisted technique, the composite membrane exhibited exceptional pervaporation performance at 30 C: concentration of water at the permeate side = 99.6 wt% and permeation flux = 2.54 kg m-2 h-1. Moreover, the membrane sustained its operating stability at a high temperature of 70 C: a high water concentration of 99.5 wt% was maintained, and a permeation flux as high as 4.34 kg m-2 h-1 was attained. This excellent separation performance stemmed from the dense, highly ordered laminate structure of GO.

Keywords: graphene oxide, self-assembly, alcohol dehydration, polyacrylonitrile (mPAN)

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Authors: Hyunchul Oh

Abstract:

One of the challenges in modern separation science and technology is the separation of hydrogen isotopes mixtures since D2 and H2 consist of almost identical size, shape and thermodynamic properties. Recently, quantum sieving of isotopes by confinement in narrow space has been proposed as an alternative technique. Despite many theoretical suggestions, however, it has been difficult to discover a feasible microporous material up to now. Among various porous materials, the novel class of microporous framework materials (COFs, ZIFs and MOFs) is considered as a promising material class for isotope sieving due to ultra-high porosity and uniform pore size which can be tailored. Hence, we investigate experimentally the fundamental correlation between D2/H2 molar ratio and pore size at optimized operating conditions by using different ultramicroporous frameworks. The D2/H2 molar ratio is strongly depending on pore size, pressure and temperature. An experimentally determined optimum pore diameter for quantum sieving lies between 3.0 and 3.4 Å which can be an important guideline for designing and developing feasible microporous frameworks for isotope separation. Afterwards, we report a novel strategy for efficient hydrogen isotope separation at technologically relevant operating pressure through the development of quantum sieving exploited by the pore aperture engineering. The strategy involves installation of flexible components in the pores of the framework to tune the pore surface.

Keywords: gas adsorption, hydrogen isotope, metal organic frameworks(MOFs), quantum sieving

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Authors: Michalina Aniola, Andrzej Katrusiak

Abstract:

4,4-Bipyridine is an important compound often used in chemical practice and more recently frequently applied for designing new metal organic framework (MoFs). Here we present a systematic high-pressure study of its hydrobromide salt. 4,4-Bipyridine hydrobromide monohydrate, 44biPyHBrH₂O, at ambient-pressure is orthorhombic, space group P212121 (phase a). Its hydrostatic compression shows that it is stable to 1.32 GPa at least. However, the recrystallization above 0.55 GPa reveals a new hidden b-phase (monoclinic, P21/c). Moreover, when the 44biPyHBrH2O is heated to high temperature the chemical reactions of this compound in methanol solution can be observed. High-pressure experiments were performed using a Merrill-Bassett diamond-anvil cell (DAC), modified by mounting the anvils directly on the steel supports, and X-ray diffraction measurements were carried out on a KUMA and Excalibur diffractometer equipped with an EOS CCD detector. At elevated pressure, the crystal of 44biPyHBrH₂O exhibits several striking and unexpected features. No signs of instability of phase a were detected to 1.32 GPa, while phase b becomes stable at above 0.55 GPa, as evidenced by its recrystallizations. Phases a and b of 44biPyHBrH2O are partly isostructural: their unit-cell dimensions and the arrangement of ions and water molecules are similar. In phase b the HOH-Br- chains double the frequency of their zigzag motifs, compared to phase a, and the 44biPyH+ cations change their conformation. Like in all monosalts of 44biPy determined so far, in phase a the pyridine rings are twisted by about 30 degrees about bond C4-C4 and in phase b they assume energy-unfavorable planar conformation. Another unusual feature of 44biPyHBrH2O is that all unit-cell parameters become longer on the transition from phase a to phase b. Thus the volume drop on the transition to high-pressure phase b totally depends on the shear strain of the lattice. Higher temperature triggers chemical reactions of 44biPyHBrH2O with methanol. When the saturated methanol solution compound precipitated at 0.1 GPa and temperature of 423 K was required to dissolve all the sample, the subsequent slow recrystallization at isochoric conditions resulted in disalt 4,4-bipyridinium dibromide. For the 44biPyHBrH2O sample sealed in the DAC at 0.35 GPa, then dissolved at isochoric conditions at 473 K and recrystallized by slow controlled cooling, a reaction of N,N-dimethylation took place. It is characteristic that in both high-pressure reactions of 44biPyHBrH₂O the unsolvated disalt products were formed and that free base 44biPy and H₂O remained in the solution. The observed reactions indicate that high pressure destabilized ambient-pressure salts and favors new products. Further studies on pressure-induced reactions are carried out in order to better understand the structural preferences induced by pressure.

Keywords: conformation, high-pressure, negative area compressibility, polymorphism

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Authors: S. M. Sadrameli, Y. Azizi

Abstract:

Lithium-ion batteries (LIBs) have shown to be one of the most reliable energy storage systems for electric cars in the recent years. Ambient temperature has a significant impact on the performance, lifetime, safety and cost of such batteries. Increasing the temperature degrade the lithium batteries more quickly while working at low-temperature environment results reducing the power and energy capability of the system. A thermal management system has been designed and setup in laboratory scale for controlling the temperature at optimum conditions using PEG-1000 with the melting point in the range of 33-40 oC as a phase change material. Aluminum plates have been installed in the PCM to increase the thermal conductivity and increasing the heat transfer rate. Experimental tests have been run at different discharge rates and ambient temperatures to investigate the effects of temperature on the efficiency of the batteries. The comparison has been made between the system of 6 batteries with and without PCM and the results show that PCM with aluminum plates decrease the surface temperature of the batteries that would result better performance and longer lifetime of the batteries.

Keywords: lithium-ion batteries, phase change materials, thermal management, temperature control

Procedia PDF Downloads 307