Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 12

Crystallization Related Publications

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

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

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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11 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, Ultrasound, Lactose, Taguchi method

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10 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: Crystallization, UV irradiation, LDPE/MMt nanocomposites, intercalation

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9 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: Crystallization, Extraction, squalene, Soxhlet.‎

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8 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: Crystallization, Lactose, spray drying, humid air

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7 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: Crystallization, experimental results, lithium bromide solution, Absorption chillers

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6 Structural and Computational Studies of N-[(2,6-Diethylphenyl) carbamothioyl]-2,2-diphenylacetamide, N-[(3 Ethylphenyl) carbamothioyl]-2,2-diphenylacetamide and 2,2-Diphenyl-N-{[2-(trifluoromethyl) phenyl]carbamothioyl}acetamide

Authors: Azhar Abdul Rahman, Ibrahim Abdul Razak, Suhana Arshad, Nur Rafikah Razali, Mohd Sukeri Mohd Yusof

Abstract:

Theoretical investigations are performed by DFT method of B3LYP/6-31G+(2d,p) and B3LYP/6-311G+(2d,p) basis sets for three carbonyl thiourea compounds, namely N-[(2,6-Diethylphenyl)carbamothioyl]-2,2-diphenylacetamide (Compound I), N-[(3-Ethylphenyl)carbamothioyl]-2,2-diphenylacetamide (Compound II) and 2,2-Diphenyl-N-{[2-(trifluoromethyl)phenyl]carbamothioyl}acetamide (Compound III). Theoretical calculations for bond parameters, harmonic vibration frequencies and isotropic chemical shifts are in good agreement with the experimental results. The calculated molecular vibrations show good correlation values, which are 0.998 and 0.999 with the experimental data. The energy gap for compounds I, II and III calculated at B3LYP/6-31G+(2d,p) basis set are 4.455866117, 4.297495791 and 4.313550514 eV respectively, while for B3LYP/6-311G+(2d,p) basis set the energy gap obtained are 4.453689205 (Compound I), 4.311373603 (Compound II) and 4.315727426 (Compound III) eV.

Keywords: Crystallization, thiourea, spectroscopic analysis, DFT studies

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5 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: Nanocomposites, Crystallization, multi-walled carbon nanotubes, poly (lactic acid)

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4 The removal of Ni, Cu and Fe from a Mixed Metal System using Sodium Hypophosphite as a Reducing Agent

Authors: Freeman Ntuli, Promise Sethembiso Ngema, Mohamed Belaid

Abstract:

The main objective of this study was to remove and recover Ni, Cu and Fe from a mixed metal system using sodium hypophosphite as a reducing agent and nickel powder as seeding material. The metal systems studied consisted of Ni-Cu, Ni-Fe and Ni-Cu-Fe solutions. A 5 L batch reactor was used to conduct experiments where 100 mg/l of each respective metal was used. It was found that the metals were reduced to their elemental form with removal efficiencies of over 80%. The removal efficiency decreased in the order Fe>Ni>Cu. The metal powder obtained contained between 97-99% Ni and was almost spherical and porous. Size enlargement by aggregation was the dominant particulate process.

Keywords: wastewater treatment, Crystallization, heavy metal removal, electroless plating

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

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

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: separation, Crystallization, Chloronitrobenzenes, eutectic

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2 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: Crystallization, glass-ceramic, non-isothermalkinetics, Avrami parameter

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1 X-ray Crystallographic Analysis of MinC N-Terminal Domain from Escherichia coli

Authors: Jun Yop An, Kyoung Ryoung Park, Jung-Gyu Lee, Hyung-Seop Youn, Jung-Yeon Kang, Gil Bu Kang, Soo Hyun Eom

Abstract:

MinC plays an important role in bacterial cell division system by inhibiting FtsZ assembly. However, the molecular mechanism of the action is poorly understood. E. coli MinC Nterminus domain was purified and crystallized using 1.4 M sodium citrate pH 6.5 as a precipitant. X-ray diffraction data was collected and processed to 2.3 Å from a native crystal. The crystal belonged to space group P212121, with the unit cell parameters a = 52.7, b = 54.0, c = 64.7 Å. Assuming the presence of two molecules in the asymmetric unit, the Matthews coefficient value is 1.94 Å3 Da-1, which corresponds to a solvent content of 36.5%. The overall structure of MinCN is observed as a dimer form through anti-parallel ß-strand interaction.

Keywords: Crystallization, cell division, MinC

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