Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 51

Search results for: crystallization

51 Carbon Dioxide Recovery by Membrane Assisted Crystallization

Authors: Wenyuan Ye, Jiuyang Lin, Patricia Luis, Bart Van der Bruggen

Abstract:

This study addresses the effect of impurities on the crystallization of Na2CO3 produced within a strategy for capturing CO2 from flue gases by alkaline absorption. A novel technology - membrane assisted crystallization - is proposed for Na2CO3 crystallization from mother liquors containing impurities. High purity of Na2CO3•10H2O crystals was obtained without impacting the performance of the mass transfer of water vapor through membranes during crystallization.

Keywords: Carbon dioxide recovery, crystal morphology, membrane crystallization, purity.

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50 The Use of Secondary Crystallization in Cement-Based Composites

Authors: Nikol Žižková, Šárka Keprdová, Rostislav Drochytka

Abstract:

The paper focuses on the study of the properties of cement-based composites produced using secondary crystallization (crystalline additive). In this study, cement mortar made with secondary crystallization was exposed to an aggressive environment and the influence of secondary crystallization on the degradation of the cementitious composite was investigated. The results indicate that the crystalline additive contributed to increasing the resistance of the cement-based composite to the attack of the selected environments (sodium sulphate solution and ammonium chloride solution).

Keywords: Secondary crystallization, cement-based composites, durability.

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49 Studying the Intercalation of Low Density Polyethylene/Clay Nanocomposites after Different UV Exposures

Authors: Samir Al-Zobaidi

Abstract:

This study attempts to understand the effect of different UV irradiation methods on the intercalation of LDPE/MMT nanocomposites, and its molecular behavior at certain isothermal crystallization temperature. Three different methods of UV exposure were employed using single composition of LDPE/MMT nanocomposites. All samples were annealed for 5 hours at a crystallization temperature of 100oC. The crystallization temperature was chosen to be at large supercooling temperature to ensure quick and complete crystallization. The raw material of LDPE consisted of two stable monoclinic and orthorhombic phases according to XRD results. The thermal behavior of both phases acted differently when UV exposure method was changed. The monoclinic phase was more dependent on the method used compared to the orthorhombic phase. The intercalation of clay, as well as, the non-isothermal crystallization temperature, has also shown a clear dependency on the type of UV exposure. A third phase that is thermally less stable was also observed. Its respond to UV irradiation was greater since it contains low molecular weight entities which make it more vulnerable to any UV exposure.

Keywords: LDPE/MMt nanocomposites, crystallization, UV irradiation, intercalation.

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48 Recycling of Sclareolide in the Crystallization Mother Liquid of Sclareolide by Adsorption and Chromatography

Authors: Xiang Li, Kui Chen, Bin Wu, Min Zhou

Abstract:

Sclareolide is made from sclareol by oxidiative synthesis and subsequent crystallization, while the crystallization mother liquor still contains 15%~30%wt of sclareolide to be reclaimed. With the reaction material of sclareol is provided as plant extract, many sorts of complex impurities exist in the mother liquor. Due to the difficulty in recycling sclareolide after solvent recovery, it is common practice for the factories to discard the mother liquor, which not only results in loss of sclareolide, but also contributes extra environmental burden. In this paper, a process based on adsorption and elution has been presented for recycling of sclareolide from mother liquor. After pretreatment of the crystallization mother liquor by HZ-845 resin to remove parts of impurities, sclareolide is adsorbed by HZ-816 resin. The HZ-816 resin loaded with sclareolide is then eluted by elution solvent. Finally, the eluent containing sclareolide is concentrated and fed into the crystallization step in the process. By adoption of the recycle from mother liquor, total yield of sclareolide increases from 86% to 90% with a stable purity of the final sclareolide products maintained.

Keywords: Sclareolide, resin, adsorption, chromatography.

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47 New SUZ-4 Zeolite Membrane from Sol-Gel Technique

Authors: P. Worathanakul, P. Kongkachuichay

Abstract:

A new SUZ-4 zeolite membrane with tetraethlyammonium hydroxide as the template was fabricated on mullite tube via hydrothermal sol-gel synthesis in a rotating autoclave reactor. The suitable synthesis condition was SiO2:Al2O3 ratio of 21.2 for 4 days at 155 °C crystallization under autogenous pressure. The obtained SUZ-4 possessed a high BET surface area of 396.4 m2/g, total pore volume at 2.611 cm3/g, and narrow pore size distribution with 97 nm mean diameter and 760 nm long of needle crystal shape. The SUZ-4 layer obtained from seeding crystallization was thicker than that of without seeds or in situ crystallization.

Keywords: Membrane, seeding, sol-gel, SUZ-4 Zeolite.

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46 Effects of FAU Zeolites on the Crystallization of Chloronitrobenzenes above the Eutectic Composition

Authors: Jeeranun Neaungjumnong, Sasikarn Yairit, Sudarat Pattanapaiboonkul, Pramoch Rangsunvigit, Santi Kulprathipanja

Abstract:

Crystallization has been used for the separation of chloronitrobenzene or CNBs, which are isomeric substances (o-, mand p-CNB) and important intermediates in chemical productions. Effects of feed composition on the crystallization of m- and p-CNB was first studied. The results conform to the binary phase diagram of m- and p-CNB. After that, effects of FAU zeolites (NaX, CaX, BaX, NaY and CaY) above the eutectic composition (63.5 and 65.0 wt% m-CNB in the feed) was also investigated. The results showed that the FAU zeolites significantly affected the precipitates, the composition of which was shifted from being rich in m-CNB to rich in p-CNB. Effects of the number of FAU zeolites on the precipitate composition was then studied. The results revealed that the precipitates from the lower number of the zeolites had higher p-CNB purity than those from the higher number of zeolite.

Keywords: Chloronitrobenzenes, crystallization, separation, eutectic

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45 Ultrasound Assisted Cooling Crystallization of Lactose Monohydrate

Authors: Sanjaykumar R. Patel, Parth R. Kayastha

Abstract:

α-lactose monohydrate is widely used in the pharmaceutical industries as an inactive substance that acts as a vehicle or a medium for a drug or other active substance. It is a byproduct of dairy industries, and the recovery of lactose from whey not only boosts the improvement of the economics of whey utilization but also causes a reduction in pollution as lactose recovery can reduce the BOD of whey by more than 80%. In the present study, levels of process parameters were kept as initial lactose concentration (30-50% w/w), sonication amplitude (20-40%), sonication time (2-6 hours), and crystallization temperature (10-20 oC) for the recovery of lactose in ultrasound assisted cooling crystallization. In comparison with cooling crystallization, the use of ultrasound enhanced the lactose recovery by 39.17% (w/w). The parameters were optimized for the lactose recovery using Taguchi Method. The optimum conditions found were initial lactose concentration at level 3 (50% w/w), amplitude of sonication at level 2 (40%), the sonication time at level 3 (6 hours), and crystallization temperature at level 1 (10 °C). The maximum recovery was found to be 85.85% at the optimum conditions. Sonication time and the initial lactose concentration were found to be significant parameters for the lactose recovery.

Keywords: Crystallization, Taguchi method, ultrasound, lactose.

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44 Non-Isothermal Kinetics of Crystallization and Phase Transformation of SiO2-Al2O3-P2O5-CaO-CaF Glass

Authors: Bogdan Il. Bogdanov, Plamen S. Pashev, Yancho H. Hristov, Dimitar P.Georgiev, Irena G. Markovska

Abstract:

The crystallization kinetics and phase transformation of SiO2.Al2O3.0,56P2O5.1,8CaO.0,56CaF2 glass have been investigated using differential thermal analysis (DTA), x-ray diffraction (XRD), and scanning electron microscopy (SEM). Glass samples were obtained by melting the glass mixture at 14500С/120 min. in platinum crucibles. The mixture were prepared from chemically pure reagents: SiO2, Al(OH)3, H3PO4, CaCO3 and CaF2. The non-isothermal kinetics of crystallization was studied by applying the DTA measurements carried out at various heating rates. The activation energies of crystallization and viscous flow were measured as 348,4 kJ.mol–1 and 479,7 kJ.mol–1 respectively. Value of Avrami parameter n ≈ 3 correspond to a three dimensional of crystal growth mechanism. The major crystalline phase determined by XRD analysis was fluorapatite (Ca(PO4)3F) and as the minor phases – fluormargarite (CaAl2(Al2SiO2)10F2) and vitlokite (Ca9P6O24). The resulting glass-ceramic has a homogeneous microstructure, composed of prismatic crystals, evenly distributed in glass phase.

Keywords: glass-ceramic, crystallization, non-isothermalkinetics, Avrami parameter

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43 Neural Network-Based Control Strategies Applied to a Fed-Batch Crystallization Process

Authors: P. Georgieva, S. Feyo de Azevedo

Abstract:

This paper is focused on issues of process modeling and two model based control strategies of a fed-batch sugar crystallization process applying the concept of artificial neural networks (ANNs). The control objective is to force the operation into following optimal supersaturation trajectory. It is achieved by manipulating the feed flow rate of sugar liquor/syrup, considered as the control input. The control task is rather challenging due to the strong nonlinearity of the process dynamics and variations in the crystallization kinetics. Two control alternatives are considered – model predictive control (MPC) and feedback linearizing control (FLC). Adequate ANN process models are first built as part of the controller structures. MPC algorithm outperforms the FLC approach with respect to satisfactory reference tracking and smooth control action. However, the MPC is computationally much more involved since it requires an online numerical optimization, while for the FLC an analytical control solution was determined.

Keywords: artificial neural networks, nonlinear model control, process identification, crystallization process

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42 Control Improvement of a C Sugar Cane Crystallization Using an Auto-Tuning PID Controller Based on Linearization of a Neural Network

Authors: S. Beyou, B. Grondin-Perez, M. Benne, C. Damour, J.-P. Chabriat

Abstract:

The industrial process of the sugar cane crystallization produces a residual that still contains a lot of soluble sucrose and the objective of the factory is to improve its extraction. Therefore, there are substantial losses justifying the search for the optimization of the process. Crystallization process studied on the industrial site is based on the “three massecuites process". The third step of this process constitutes the final stage of exhaustion of the sucrose dissolved in the mother liquor. During the process of the third step of crystallization (Ccrystallization), the phase that is studied and whose control is to be improved, is the growing phase (crystal growth phase). The study of this process on the industrial site is a problem in its own. A control scheme is proposed to improve the standard PID control law used in the factory. An auto-tuning PID controller based on instantaneous linearization of a neural network is then proposed.

Keywords: Auto-tuning, PID, Instantaneous linearization, Neural network, Non linear process, C-crystallisation.

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41 Application of Feed Forward Neural Networks in Modeling and Control of a Fed-Batch Crystallization Process

Authors: Petia Georgieva, Sebastião Feyo de Azevedo

Abstract:

This paper is focused on issues of nonlinear dynamic process modeling and model-based predictive control of a fed-batch sugar crystallization process applying the concept of artificial neural networks as computational tools. The control objective is to force the operation into following optimal supersaturation trajectory. It is achieved by manipulating the feed flow rate of sugar liquor/syrup, considered as the control input. A feed forward neural network (FFNN) model of the process is first built as part of the controller structure to predict the process response over a specified (prediction) horizon. The predictions are supplied to an optimization procedure to determine the values of the control action over a specified (control) horizon that minimizes a predefined performance index. The control task is rather challenging due to the strong nonlinearity of the process dynamics and variations in the crystallization kinetics. However, the simulation results demonstrated smooth behavior of the control actions and satisfactory reference tracking.

Keywords: Feed forward neural network, process modelling, model predictive control, crystallization process.

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40 Effect of Humidity on in-Process Crystallization of Lactose during Spray Drying

Authors: Amirali Ebrahimi, T. A. G. Langrish

Abstract:

The effect of various humidities on process yields and degrees of crystallinity for spray-dried powders from spray drying of lactose with humid air in a straight-through system have been studied. It has been suggested by Williams–Landel–Ferry kinetics (WLF) that a higher particle temperature and lower glass-transition temperature would increase the crystallization rate of the particles during the spray-drying process. Freshly humidified air produced by a Buchi-B290 spray dryer as a humidifier attached to the main spray dryer decreased the particle glass-transition temperature (Tg), while allowing the particle temperature (Tp) to reach higher values by using an insulated drying chamber. Differential scanning calorimetry (DSC) and moisture sorption analysis were used to measure the degree of crystallinity for the spray-dried lactose powders. The results showed that higher Tp-Tg, as a result of applying humid air, improved the process yield from 21 ± 4 to 26 ± 2% and crystallinity of the particles by decreasing the latent heat of crystallization from 43 ± 1 to 30 ± 11 J/g and the sorption peak height from 7.3 ± 0.7% to 6 ± 0.7%.

Keywords: Lactose, crystallization, spray drying, humid air.

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39 Thermal Stability and Crystallization Behaviour of Modified ABS/PP Nanocomposites

Authors: Marianna I. Triantou, Petroula A. Tarantili

Abstract:

In this research work, poly (acrylonitrile-butadienestyrene)/ polypropylene (ABS/PP) blends were processed by melt compounding in a twin-screw extruder. Upgrading of the thermal characteristics of the obtained materials was attempted by the incorporation of organically modified montmorillonite (OMMT), as well as, by the addition of two types of compatibilizers; polypropylene grafted with maleic anhydride (PP-g-MAH) and ABS grafted with maleic anhydride (ABS-g-MAH). The effect of the above treatments was investigated separately and in combination. Increasing the PP content in ABS matrix seems to increase the thermal stability of their blend and the glass transition temperature (Tg) of SAN phase of ABS. From the other part, the addition of ABS to PP promotes the formation of its β-phase, which is maximum at 30 wt% ABS concentration, and increases the crystallization temperature (Tc) of PP. In addition, it increases the crystallization rate of PP.The β-phase of PP in ABS/PP blends is reduced by the addition of compatibilizers or/and organoclay reinforcement. The incorporation of compatibilizers increases the thermal stability of PP and reduces its melting (ΔΗm) and crystallization (ΔΗc) enthalpies. Furthermore it decreases slightly the Tgs of PP and SAN phases of ABS/PP blends. Regarding the storage modulus of the ABS/PP blends, it presents a change in their behavior at about 10°C and return to their initial behavior at ~110°C. The incorporation of OMMT to no compatibilized and compatibilized ABS/PP blends enhances their storage modulus.

Keywords: Acrylonitrile, butadiene, styrene terpolymer, compatibilizer, organoclay, polypropylene.

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38 Model based Soft-Sensor for Industrial Crystallization: On-line Mass of Crystals and Solubility Measurement

Authors: Cédric Damour, Michel Benne, Brigitte Grondin-Perez, Jean-Pierre Chabriat

Abstract:

Monitoring and control of cane sugar crystallization processes depend on the stability of the supersaturation (σ ) state. The most widely used information to represent σ is the electrical conductivity κ of the solutions. Nevertheless, previous studies point out the shortcomings of this approach: κ may be regarded as inappropriate to guarantee an accurate estimation of σ in impure solutions. To improve the process control efficiency, additional information is necessary. The mass of crystals in the solution ( c m ) and the solubility (mass ratio of sugar to water / s w m m ) are relevant to complete information. Indeed, c m inherently contains information about the mass balance and / s w m m contains information about the supersaturation state of the solution. The main problem is that c m and / s w m m are not available on-line. In this paper, a model based soft-sensor is presented for a final crystallization stage (C sugar). Simulation results obtained on industrial data show the reliability of this approach, c m and the crystal content ( cc ) being estimated with a sufficient accuracy for achieving on-line monitoring in industry

Keywords: Soft-sensor, on-line monitoring, cane sugarcrystallization.

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37 Mineral Chemistry and Petrography of Lava Successions From Kepsut-Dursunbey Volcanic Field, NW Turkey: Implications For Magmatic Processes and Crystallization Conditions

Authors: Kamaci O., Altunkaynak S.

Abstract:

Kepsut-Dursunbey volcanic field (KDVF) is located in NW Turkey and contains various products of the post-collisional Neogene magmatic activity. Two distinct volcanic suites have been recognized; the Kepsut volcanic suite (KVS) and the Dursunbey volcanic suite (DVS). The KVS includes basaltic trachyandesitebasaltic andesite-andesite lavas and associated pyroclastic rocks. The DVS consists of dacite-rhyodacite lavas and extensive pumice-ash fall and flow deposits. Petrographical features (i.e. existence of xenocrysts, glomerocrysts, and mixing-compatible textures) and mineral chemistry of phenocryst assemblages of both suites provide evidence for magma mixing/AFC. Calculated crystallization pressures and temperatures give values of 5.7–7.0 kbar and 927–982 °C for the KVS and 3.7–5.3 kbar and 783-787°C for the DVS, indicating separate magma reservoirs and crystallization in magma chambers at deep and mid crustal levels, respectively. These observations support the establishment and evolution of KDVF magma system promoted by episodic basaltic inputs which may generate and mix with crustal melts.

Keywords: mineral chemistry, mixing, basaltic inputs, NW Turkey

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36 Extraction of Squalene from Lebanese Olive Oil

Authors: Henri El Zakhem, Christina Romanos, Charlie Bakhos, Hassan Chahal, Jessica Koura

Abstract:

Squalene is a valuable component of the oil composed of 30 carbon atoms and is mainly used for cosmetic materials. The main concern of this article is to study the Squalene composition in the Lebanese olive oil and to compare it with foreign oil results. To our knowledge, extraction of Squalene from the Lebanese olive oil has not been conducted before. Three different techniques were studied and experiments were performed on three brands of olive oil, Al Wadi Al Akhdar, Virgo Bio and Boulos. The techniques performed are the Fractional Crystallization, the Soxhlet and the Esterification. By comparing the results, it is found that the Lebanese oil contains squalene and Soxhlet method is the most effective between the three methods extracting about 6.5E-04 grams of Squalene per grams of olive oil.

Keywords: Squalene, extraction, crystallization, Soxhlet.‎

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35 Impact of Fluid Flow Patterns on Metastable Zone Width of Borax in Dual Radial Impeller Crystallizer at Different Impeller Spacings

Authors: A. Čelan, M. Ćosić, D. Rušić, N. Kuzmanić

Abstract:

Conducting crystallization in an agitated vessel requires a proper selection of mixing parameters that would result in a production of crystals of specific properties. In dual impeller systems, which are characterized by a more complex hydrodynamics due to the possible fluid flow interactions, revealing a clear link between mixing parameters and crystallization kinetics is still an open issue. The aim of this work is to establish this connection by investigating how fluid flow patterns, generated by two impellers mounted on the same shaft, reflect on metastable zone width of borax decahydrate, one of the most important parameters of the crystallization process. Investigation was carried out in a 15-dm3 bench scale batch cooling crystallizer with an aspect ratio (H/T) equal to 1.3. For this reason, two radial straight blade turbines (4-SBT) were used for agitation. Experiments were conducted at different impeller spacings at the state of complete suspension. During the process of an unseeded batch cooling crystallization, solution temperature and supersaturation were continuously monitored what enabled a determination of the metastable zone width. Hydrodynamic conditions in the vessel achieved at different impeller spacings investigated were analyzed in detail. This was done firstly by measuring the mixing time required to attain the desired level of homogeneity. Secondly, fluid flow patterns generated in a described dual impeller system were both photographed and simulated by VisiMix Turbulent software. Also, a comparison of these two visualization methods was performed. Experimentally obtained results showed that metastable zone width is definitely affected by the hydrodynamics in the crystallizer. This means that this crystallization parameter can be controlled not only by adjusting the saturation temperature or cooling rate, as is usually done, but also by choosing a suitable impeller spacing that will result in a formation of crystals of wanted size distribution.

Keywords: Dual impeller crystallizer, fluid flow pattern, metastable zone width, mixing time, radial impeller.

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34 Deformation and Crystallization in a 7075-T651 Friction Stir Weld

Authors: C. S. Paglia

Abstract:

The deformation and the crystallization in a 7075-T651 friction stir weld, in particular for regions directly in contact with the mechanical action of the rotating probe, have been investigated by means of optical microscopy. The investigation enabled to identify regions of the weld differently affected by the deformation caused by the welding process. The highly deformed grains in the horizontal direction close to the plate margin were indicative of shear movements along the horizontal plane, while highly deformed grains along the plate margin in the vertical direction were indicative of vertical shear movements of opposite directions, which superimposed the shear movement along the horizontal plane. The vertical shear movements were not homogeneous through the plate thickness. The microstructure indicated that after the probe passes, the grain growth may take place under static conditions. The small grains microstructure of the nugget region, formed after the main dynamic recrystallization process, develops to an equiaxed microstructure. A material transport influenced by the rotating shoulder was also observed from the trailing to the advancing side of the weld.

Keywords: AA7075-T651, friction stir welding, deformation, crystallization.

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33 An Automated High Pressure Differential Thermal Analysis System for Phase Transformation Studies

Authors: T. K. Mondal, N C Shivaprakash

Abstract:

A piston cylinder based high pressure differential thermal analyzer system is developed to investigate phase transformations, melting, glass transitions, crystallization behavior of inorganic materials, glassy systems etc., at ambient to 4 GPa and at room temperature to 1073 K. The pressure is calibrated by the phase transition of bismuth and ytterbium and temperature is calibrated by using thermocouple data chart. The system developed is calibrated using benzoic acid, ammonium nitrate and it has a pressure and temperature control of ± 8.9 x 10 -4 GPa , ± 2 K respectively. The phase transition of Asx Te100-x chalcogenides, ferrous oxide and strontium boride are studied using the indigenously developed system.

Keywords: double stage crystallization, Phase transition, Quasi hydrostatic, Rigidity percolation

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32 Characterization of Biodegradable Nanocomposites with Poly (Lactic Acid) and Multi-Walled Carbon Nanotubes

Authors: Md F. Mina, Mohammad D.H. Beg, Muhammad R. Islam, Abu K. M. M. Alam A. Nizam, Rosli M. Younus

Abstract:

In this study, structural, mechanical, thermal and electrical properties of poly (lactic acid) (PLA) nanocomposites with low-loaded (0-1.5 wt%) untreated, heat and nitric acid treated multiwalled carbon nanotubes (MWCNTs) were studied. Among the composites, untreated 0.5 wt % MWCNTs and acid-treated 1.0 wt% MWCNTs reinforced PLA show the tensile strength and modulus values higher than the others. These two samples along with pure PLA exhibit the stable orthorhombic α-form, whilst other samples reveal the less stable orthorhombic β-form, as demonstrated by X-ray diffraction study. Differential scanning calorimetry reveals the evolution of the mentioned different phases by controlled cooling and discloses an enhancement of PLA crystallization by nanotubes incorporation. Thermogravimetric analysis shows that the MWCNTs loaded sample degraded faster than PLA. Surface resistivity of the nanocomposites is found to be dropped drastically by a factor of 1013 with a low loading of MWCNTs (1.5 wt%).

Keywords: Crystallization, multi-walled carbon nanotubes, nanocomposites, Poly (lactic acid).

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31 Effect of Si/Al Ratio on SSZ-13 Crystallization and Its Methanol-To-Olefins Catalytic Properties

Authors: Zhiqiang Xu, Hongfang Ma, Haitao Zhang, Weixin Qian, Weiyong Ying

Abstract:

SSZ-13 materials with different Si/Al ratio were prepared by varying the composition of aluminosilicate precursor solutions upon hydrothermal treatment at 150 °C. The Si/Al ratio of the initial system was systematically changed from 12.5 to infinity in order to study the limits of Al composition in precursor solutions for constructing CHA structure. The intermediates and final products were investigated by complementary techniques such as XRD, HRTEM, FESEM, and chemical analysis. NH3-TPD was used to study the Brønsted acidity of SSZ-13 samples with different Si/Al ratios. The effect of the Si/Al ratio on the precursor species, ultimate crystal size, morphology and yield was investigated. The results revealed that Al species determine the nucleation rate and the number of nuclei, which is tied to the morphology and yield of SSZ-13. The size of SSZ-13 increased and the yield decreased as the Si/Al ratio was improved. Varying Si/Al ratio of the initial system is a facile, commercially viable method of tailoring SSZ-13 crystal size and morphology. Furthermore, SSZ-13 materials with different Si/Al ratio were tested as catalysts for the methanol to olefins (MTO) reaction at 350 °C. SSZ-13 with the Si/Al ratio of 35 shows the best MTO catalytic performance.

Keywords: Crystallization, MTO, Si/Al ratio, SSZ-13.

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30 Carbamazepine Co-crystal Screening with Dicarboxylic Acids Co-Crystal Formers

Authors: Syarifah Abd Rahim, Fatinah Ab Rahman, Engku N. E. M. Nasir, Noor A. Ramle

Abstract:

Co-crystal is believed to improve the solubility and dissolution rates and thus, enhanced the bioavailability of poor water soluble drugs particularly during the oral route of administration. With the existing of poorly soluble drugs in pharmaceutical industry, the screening of co-crystal formation using carbamazepine (CBZ) as a model drug compound with dicarboxylic acids co-crystal formers (CCF) namely fumaric (FA) and succinic (SA) acids in ethanol has been studied. The co-crystal formations were studied by varying the mol ratio values of CCF to CBZ to access the effect of CCF concentration on the formation of the co-crystal. Solvent evaporation, slurry and cooling crystallization which representing the solution based method co-crystal screening were used. Based on the differential scanning calorimetry (DSC) analysis, the melting point of CBZ-SA in different ratio was in the range between 188oC-189oC. For CBZ-FA form A and CBZ-FA form B the melting point in different ratio were in the range of 174oC-175oC and 185oC-186oC respectively. The product crystal from the screening was also characterized using X-ray powder diffraction (XRPD). The XRPD pattern profile analysis has shown that the CBZ co-crystals with FA and SA were successfully formed for all ratios studied. The findings revealed that CBZ-FA co-crystal were formed in two different polymorphs. It was found that CBZ-FA form A and form B were formed from evaporation and slurry crystallization methods respectively. On the other hand, in cooling crystallization method, CBZ-FA form A was formed at lower mol ratio of CCF to CBZ and vice versa. This study disclosed that different methods and mol ratios during the co-crystal screening can affect the outcome of co-crystal produced such as polymorphic forms of co-crystal and thereof. Thus, it was suggested that careful attentions is needed during the screening since the co-crystal formation is currently one of the promising approach to be considered in research and development for pharmaceutical industry to improve the poorly soluble drugs.

Keywords: Carbamazepine, co-crystal, co-crystal former, dicarboxylic acid.

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29 Thermal and Mechanical Properties of Modified CaCO3 /PP Nanocomposites

Authors: A. Buasri, N. Chaiyut, K. Borvornchettanuwat, N. Chantanachai, K. Thonglor

Abstract:

Inorganic nanoparticles filled polymer composites have extended their multiple functionalities to various applications, including mechanical reinforcement, gas barrier, dimensional stability, heat distortion temperature, flame-retardant, and thermal conductivity. Sodium stearate-modified calcium carbonate (CaCO3) nanoparticles were prepared using surface modification method. The results showed that sodium stearate attached to the surface of CaCO3 nanoparticles with the chemical bond. The effect of modified CaCO3 nanoparticles on thermal properties of polypropylene (PP) was studied by means of differential scanning calorimetry (DSC) and Thermogravimetric analysis (TGA). It was found that CaCO3 significantly affected the crystallization temperature and crystallization degree of PP. Effect of the modified CaCO3 content on mechanical properties of PP/CaCO3 nanocomposites was also studied. The results showed that the modified CaCO3 can effectively improve the mechanical properties of PP. In comparison with PP, the impact strength of PP/CaCO3 nanocomposites increased by about 65% and the hardness increased by about 5%.

Keywords: Polypropylene Nanocomposites, Modified Calcium Carbonate, Sodium Stearate, Surface Treatment

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28 Effectiveness of Crystallization Coating Materials on Chloride Ions Ingress in Concrete

Authors: Mona Elsalamawy, Ashraf Ragab Mohamed, Abdellatif Elsayed Abosen

Abstract:

This paper aims to evaluate the effectiveness of different crystalline coating materials concerning of chloride ions penetration. The concrete ages at the coating installation and its moisture conditions were addressed; where, these two factors may play a dominant role for the effectiveness of the used materials. Rapid chloride ions penetration test (RCPT) was conducted at different ages and moisture conditions according to the relevant standard. In addition, the contaminated area and the penetration depth of the chloride ions were investigated immediately after the RCPT test using chemical identifier, 0.1 M silver nitrate AgNO3 solution. Results have shown that, the very low chloride ions penetrability, for the studied crystallization materials, were investigated only with the old age concrete (G1). The significant reduction in chloride ions’ penetrability was illustrated after 7 days of installing the crystalline coating layers. Using imageJ is more reliable to describe the contaminated area of chloride ions, where the distribution of aggregate and heterogeneous of cement mortar was considered in the images analysis.

Keywords: Chloride permeability, contaminated area, crystalline waterproofing materials, RCPT, XRD.

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27 The Experimental Measurement of the LiBr Concentration of a Solar Absorption Machine

Authors: N. Hatraf, L. Merabeti, Z. Neffeh, W. Taane

Abstract:

The excessive consumption of fossil energies (electrical energy) during summer caused by the technological development involves more and more climate warming.

In order to reduce the worst impact of gas emissions produced from classical air conditioning, heat driven solar absorption chiller is pretty promising; it consists on using solar as motive energy which is clean and environmentally friendly to provide cold.

Solar absorption machine is composed by four components using Lithium Bromide /water as a refrigerating couple. LiBr- water is the most promising in chiller applications due to high safety, high volatility ratio, high affinity, high stability and its high latent heat. The lithium bromide solution is constitute by the salt lithium bromide which absorbs water under certain conditions of pressure and temperature however if the concentration of the solution is high in the absorption chillers; which exceed 70%, the solution will crystallize.

The main aim of this article is to study the phenomena of the crystallization and to evaluate how the dependence between the electric conductivity and the concentration which should be controlled.

Keywords: Absorption chillers, crystallization, experimental results, Lithium Bromide solution.

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26 Jalovchat Gabbroic Intrusive of the Caucasus: Petrological Study, Geochemical Peculiarities and Formation Conditions

Authors: Giorgi Chichinadze, David Shengelia, Tamara Tsutsunava, Nikoloz Maisuradze, Giorgi Beridze

Abstract:

The Jalovchat intrusive is built up of hornblende gabbros, gabbro-norites and norites. Within the intrusive hornblende-bearing gabbro-pegmatites are widespread. That is a coarse-grained rock with gigantic hornblende crystals. By its unusual composition, the Jalovchat intrusive has no analogue in the Caucasus. However, petrologically and geochemically, the intrusive rocks were studied insufficiently. For comprehensive investigations, the authors applied appropriate methodologies: Microscopic study of thin sections, petro- and geochemical analyses of the samples and also different petrogenic, rare and rare earth elements diagrams and spidergrams. Analytical study established that the Jalovchat intrusive by its composition corresponds mainly to the mid-ocean ridge basalts and according to geodynamic type belongs to the subduction type. In general, it is an anomalous phenomenon, as in the rocks of such composition crystallization of hornblende and especially of its gigantic crystals is atypical. The authors believe that the water-rich magma reservoir, which was necessary for the crystallization of gigantic hornblende crystals, appeared as a result of melting of water-rich mid-ocean ridge basaltic rocks during the subduction process in Bajocian time.

Keywords: Gabbroic intrusive, petrology, geochemistry, genesis, the Caucasus.

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25 Experimental Investigation on Freeze-Concentration Process Desalting for Highly Saline Brines

Authors: H. Al-Jabli

Abstract:

Using the freeze-melting process for the disposing of high saline brines was the aim of the paper by confirming the performance estimation of the treatment system. A laboratory bench scale freezing technique test unit was designed, constructed, and tested at Doha Research Plant (DRP) in Kuwait. The principal unit operations that have been considered for the laboratory study are: ice crystallization, separation, washing, and melting. The applied process is characterized as “the secondary-refrigerant indirect freezing”, which is utilizing normal freezing concept. The high saline brine was used as definite feed water, i.e. average TDS of 250,000 ppm. Kuwait desalination plants were carried out in the experimental study to measure the performance of the proposed treatment system. Experimental analysis shows that the freeze-melting process is capable of dropping the TDS of the feed water from 249,482 ppm to 56,880 ppm of the freeze-melting process in the two-phase’s course, whereas overall recovery results of the salt passage and salt rejection are 31.11%, 19.05%, and 80.95%, correspondingly. Therefore, the freeze-melting process is encouraging for the proposed application, as it shows on the results, which approves the process capability of reducing a major amount of the dissolved salts of the high saline brine with reasonable sensible recovery. This process might be reasonable with other brine disposal processes.

Keywords: High saline brine, freeze-melting process, ice crystallization, brine disposal process.

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24 Impact of Mixing Parameters on Homogenization of Borax Solution and Nucleation Rate in Dual Radial Impeller Crystallizer

Authors: A. Kaćunić, M. Ćosić, N. Kuzmanić

Abstract:

Interaction between mixing and crystallization is often ignored despite the fact that it affects almost every aspect of the operation including nucleation, growth, and maintenance of the crystal slurry. This is especially pronounced in multiple impeller systems where flow complexity is increased. By choosing proper mixing parameters, what closely depends on the knowledge of the hydrodynamics in a mixing vessel, the process of batch cooling crystallization may considerably be improved. The values that render useful information when making this choice are mixing time and power consumption. The predominant motivation for this work was to investigate the extent to which radial dual impeller configuration influences mixing time, power consumption and consequently the values of metastable zone width and nucleation rate. In this research, crystallization of borax was conducted in a 15 dm3 baffled batch cooling crystallizer with an aspect ratio (H/T) of 1.3. Mixing was performed using two straight blade turbines (4-SBT) mounted on the same shaft that generated radial fluid flow. Experiments were conducted at different values of N/NJS ratio (impeller speed/ minimum impeller speed for complete suspension), D/T ratio (impeller diameter/crystallizer diameter), c/D ratio (lower impeller off-bottom clearance/impeller diameter), and s/D ratio (spacing between impellers/impeller diameter). Mother liquor was saturated at 30°C and was cooled at the rate of 6°C/h. Its concentration was monitored in line by Na-ion selective electrode. From the values of supersaturation that was monitored continuously over process time, it was possible to determine the metastable zone width and subsequently the nucleation rate using the Mersmann’s nucleation criterion. For all applied dual impeller configurations, the mixing time was determined by potentiometric method using a pulse technique, while the power consumption was determined using a torque meter produced by Himmelstein & Co. Results obtained in this investigation show that dual impeller configuration significantly influences the values of mixing time, power consumption as well as the metastable zone width and nucleation rate. A special attention should be addressed to the impeller spacing considering the flow interaction that could be more or less pronounced depending on the spacing value.

Keywords: Dual impeller crystallizer, mixing time, power consumption, metastable zone width, nucleation rate.

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23 Geochemistry of Cenozoic Basaltic Rocksaround Liuhe National Geopark, Jiangsu Province, Eastern China: Petrogenesis and Mantle Source

Authors: Yung-Tan Lee, Ren-Yi Huang, Ju-Chin Chen, Jyh-Yi Shih, Meng-Lung Lin, Hsiao-Ling Yu, Yen-Tsui Hu, Chih-Cheng Chen

Abstract:

Cenozoic basalts found in Jiangsu province of eastern China include tholeiites and alkali basalts. The present paper analyzed the major, trace elements, rare earth elements of these Cenozoic basalts and combined with Sr-Nd isotopic compositions proposed by Chen et al. (1990)[1] in the literatures to discuss the petrogenesis of these basalts and the geochemical characteristics of the source mantle. Based on major, trace elements and fractional crystallization model established by Brooks and Nielsen (1982)[2] we suggest that the basaltic magma has experienced olivine + clinopyroxene fractionation during its evolution. The chemical compositions of basaltic rocks from Jiangsu province indicate that these basalts may belong to the same magmatic system. Spidergrams reveal that Cenozoic basalts from Jiangsu province have geochemical characteristics similar to those of ocean island basalts(OIB). The slight positive Nb and Ti anomalies found in basaltic rocks of this study suggest the presence of Ti-bearing minerals in the mantle source and these Ti-bearing minerals had contributed to basaltic magma during partial melting, indicating a metasomatic event might have occurred before the partial melting. Based on the Sr vs. Nd isotopic ratio plots, we suggest that Jiangsu basalts may be derived from partial melting of mantle source which may represent two-end members mixing of DMM and EM-I. Some Jiangsu basaltic magma may be derived from partial melting of EM-I heated by the upwelling asthenospheric mantle or asthenospheric diapirism.

Keywords: Geochemistry, Jiangsu Province, Cenozoic basalts, Fractional crystallization.

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22 Volatile Organic Compounds Destruction by Catalytic Oxidation for Environmental Applications

Authors: Mohammed Nasir Kajama, Ngozi Claribelle Nwogu, Edward Gobina

Abstract:

Pt/γ-Al2O3 membrane catalysts were prepared via an evaporative-crystallization deposition method. The obtained Pt/γ- Al2O3 catalyst activity was tested after characterization (SEM-EDAX observation, BET measurement, permeability assessment) in the catalytic oxidation of selected volatile organic compound (VOC) i.e. propane, fed in mixture of oxygen. The VOC conversion (nearly 90%) obtained by varying the operating temperature showed that flow-through membrane reactor might do better in the abatement of VOCs.

Keywords: VOC combustion, flow-through membrane reactor, platinum supported alumina catalysts.

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