Search results for: reversible addition−fragmentation chain-transfer polymerization

Authors: Tsung-Yen Tsai, Naveen Bunekar, Ming Hsuan Chang, Wen-Kuang Wang, Satoshi Onda

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The structure-property relationship and initiator effect on bulk polymerized poly(methyl methacrylate) (PMMA)–oragnomodified layered silicate nanocomposites was investigated. In this study, we used 2, 2'-azobis (4-methoxy-2,4-dimethyl valeronitrile and benzoyl peroxide initiators for bulk polymerization. The bulk polymerized nanocomposites’ morphology was investigated by X-ray diffraction and transmission electron microscopy. The type of initiator strongly influences the physiochemical properties of the polymer nanocomposite. The thermal degradation of PMMA in the presence of nanofiller was studied. 5 wt% weight loss temperature (T5d) increased as compared to pure PMMA. The peak degradation temperature increased for the nanocomposites. Differential scanning calorimetry and dynamic mechanical analysis were performed to investigate the glass transition temperature and the nature of the constrained region as the reinforcement mechanism respectively. Furthermore, the optical properties such as UV-Vis and Total Luminous Transmission of nanocomposites are examined.

Keywords: initiator, bulk polymerization, layered silicates, methyl methacrylate

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Authors: Y. Jeon, A. Bissessur, J. Lin, P. Ndungu

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Most transformers employ the usage of cellulose paper, which has been chemically modified through the Kraft process that acts as an effective insulator. Cellulose ageing and oil degradation are directly linked to fouling of the transformer and accumulation of large quantities of waste insulating paper. In addition to technical difficulties, this proves costly for power utilities to deal with. Currently there are no cost effective method for the rejuvenation of cellulose paper that has been documented nor proposed, since renewal of used insulating paper is implemented as the best option. This study proposes and contrasts different rejuvenation methods of accelerated aged cellulose insulating paper by chemical and bio-bleaching processes. Of the three bleaching methods investigated, two are, conventional chlorine-based sodium hypochlorite (m/v), and chlorine-free hydrogen peroxide (v/v), whilst the third is a bio-bleaching technique that uses a bacterium isolate, Acinetobacter strain V2. Through chemical bleaching, varying the strengths of the bleaching reagents at 0.3 %, 0.6 %, 0.9 %, 1.2 %, 1.5 % and 1.8 % over 4 hrs. were analyzed. Bio-bleaching implemented a bacterium isolate, Acinetobacter strain V2, to bleach the aged Kraft paper over 4 hrs. The determination of the amount of alpha cellulose, degree of polymerization and viscosity carried out on Kraft-cellulose insulating paper before and after bleaching. Overall the investigated techniques of chemical and bio-bleaching were successful and effective in treating degraded and accelerated aged Kraft-cellulose insulating paper, however, to varying extents. Optimum conditions for chemical bleaching were attained at bleaching strengths of 1.2 % (m/v) NaOCl and 1.5 % (v/v) H2O2 yielding alpha cellulose contents of 82.4 % and 80.7 % and degree of polymerizations of 613 and 616 respectively. Bio-bleaching using Acinetobacter strain V2 proved to be the superior technique with alpha cellulose levels of 89.0 % and a degree of polymerization of 620. Chemical bleaching techniques require careful and controlled clean-up treatments as it is chlorine and hydrogen peroxide based while bio-bleaching is an extremely eco-friendly technique.

Keywords: alpha cellulose, bio-bleaching, degree of polymerization, Kraft-cellulose insulating paper, transformer, viscosity

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Authors: Elmira Ghanbari, Jan Van Esch, Stephen J. Picken, Sahil Aggarwal

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Organogels are formed by the assembly of low molecular weight gelators (LMWG) into fibrous structures. The assembly of these molecules into crystalline fibrous structures occurs as a result of reversible interactions such as π-stacking, hydrogen-bonding, and van der Waals interactions. Bisamide organogelators with two amide groups have been used as one of LMWGs which show efficient assembly behavior via hydrogen bonding for network formation, the formation of a crystalline network for solvent entrapment. In this study, different bisamide gelators with different lengths of alkyl chains have been added to the bisamide parent gels. The effect of the addition of bisamide additives on the gelation of bisamide gels is described. Investigation of the thermal properties of the gels by differential scanning calorimetry and dropping ball techniques indicated that the bisamide gels can be formed by the addition of a high concentration of the second bisamide components. The microstructure of the gels with different gelator components has been visualized with scanning electron microscopy (SEM) which has shown systematic woven, platelet-like, and a combination of those morphologies for different gels. Examining the addition of a range of bisamide additives with different structural characteristics than the parent bisamide gels has confirmed the effect of the molecular structure on the morphology of the bisamide gels and their final properties.

Keywords: bisamide organogelator additives, gel morphology, gel properties, self-assembly

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Authors: Fatima Zohra Zeggai, Benjamin Carbonnier, Aïcha Hachemaoui, Ahmed Yahiaoui, Samia Mahouche-Chergui, Zakaria Salmi

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A series of polyaniline (PANI)/modified Montmorillonite (MMT) Clay nanocomposite materials have been successfully prepared by In-Situ polymerization in the presence of modified MMT-Clay or Diazonium-MMT-Clay. The obtained nanocomposites were characterized and compared by various physicochemical techniques. The presence of physicochemical interaction, probably hydrogen bonding, between clay and polyaniline, which was confirmed by FTIR, UV-Vis Spectroscopy. The electrical conductivity of neat PANI and a series of the obtained nanocomposites were also studied by cyclic voltammograms.

Keywords: polyaniline, clay, nanocomposites, in-situ polymerization, polymers conductors, diazonium salt

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Authors: Fatma Zehra Engin Sagirli, Eyup Sabri Kayali, A. Sezai Sarac

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In this study, Poly (acrylonitrile-co-methylacrylate)/N-Methyl Pyrrole and Pyrrole ([P(AN-co-MA)]-NMPy and [P(AN-co-MA)]-PPy) core–shell nanoparticles were obtained by in situ emulsion polymerization in the presence of Sodium dodecyl benzene sulfonate and sodium dodecyl sulfate (SDBS and SDS) by using ammonium per sulphate in the aqueous medium. The spectroscopic characterizations during the formation of nanocomposites were studied using Attenuated total reflectance Fourier transform infrared (FTIR-ATR) spectroscopy, ultraviolet–visible spectrophotometer (Uv-Vis). Electrical conductivity of the emulsion solution was measured by Conductivity Meter from aqueous sample solution. Also, yield of the powder nanocomposites was measured. SDBS and SDS used for investigation of surfactant effect on yield, electrical conductivity and polymerization process. Determination of polymerization yield, (FTIR-ATR) and (Uv-Vis) prove that the SDBS surfactant become more incorporated into the conducting polymers and there is strong interaction between the [P(AN-co-MA)]-PPy derivatives which prepared by these surfactants. The similar inclusion of SDS into conducting polymers was not observed, there is a remarkable difference at nanocomposites which prepared with SDS.

Keywords: nanocomposites, core-shell, pyrole, surfactant

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Authors: S. Padmapriya, V. Lakshmi Prabha

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In this paper, an efficient reconfigurable fixed-point Least Mean Square Adaptive FIR filter is proposed. The proposed architecture has two methods of operation: one is area efficient design and the other is optimized power. Pipelining of the adder blocks and partial product generator are used to achieve low area and reversible logic is used to obtain low power design. Depending upon the input samples and filter coefficients, one of the techniques is chosen. Least-Mean-Square adaptation is performed to update the weights. The architecture is coded using Verilog and synthesized in cadence encounter 0.18μm technology. The synthesized results show that the area reduction ratio of the proposed when compared with conventional technique is about 1.2%.

Keywords: adaptive filter, carry select adder, least mean square algorithm, reversible logic

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Authors: Vipin Saini, Manish Kumar, Shailendra Bhatt, A. Pandurangan

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The aim of the present study was to fabricate a thermo sensitive gel containing Chlorpheniramine maleate (CPM) loaded nanoparticles following intranasal administration for effective treatment of allergic rhinitis. Chitosan based nanoparticles were prepared by precipitation method followed by the addition of developed NPs within the Poloxamer 407 and carbopol 934P based mucoadhesive thermo-reversible gel. Developed formulations were evaluated for Particle size, PDI, % entrapment efficiency and % cumulative drug permeation. NP3 formulation was found to be optimized on the basis of minimum particle size (143.9 nm), maximum entrapment efficiency (80.10±0.414 %) and highest drug permeation (90.92±0.531 %). The optimized formulation NP3 was then formulated into thermo reversible in situ gel. This intensifies the contact between nasal mucosa and the drug, increases and facilitates the drug absorption which results in increased bioavailability. G4 formulation was selected as the optimize on the basis of gelation ability and mucoadhesive strength. Histology was carried out to examine the damage caused by the optimized G4 formulation. Results revealed no visual signs of tissue damage thus indicated safe nasal delivery of nanoparticulate in situ gel formulation G4. Thus, intranasal CPM NP-loaded in situ gel was found to be a promising formulation for the treatment of allergic rhinitis.

Keywords: chitosan, nanoparticles, in situ gel, chlorpheniramine maleate, poloxamer 407

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Authors: Imam Wierawansyah Eltara, Iftitah, Agus Ismail

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In the present work, cellulose nanowhiskers (CNW) extracted from coconut husk fibers, were incorporated in polylactide (PLA)-based composites. Prior to the blending, PLA chains were chemically grafted on the surface of CNW to enhance the compatibilization between CNW and the hydrophobic polyester matrix. Ring-opening polymerization of L-lactide was initiated from the hydroxyl groups available at the CNW surface to yield CNW-g-PLA nanohybrids. PLA-based nanocomposites were prepared by melt blending to ensure a green concept of the study thereby limiting the use of organic solvents. The influence of PLA-grafted cellulose nanoparticles on the mechanical and thermal properties of the ensuing nanocomposites was deeply investigated. The thermal behavior and mechanical properties of the nanocomposites were determined using differential scanning calorimetry (DSC) and dynamical mechanical and thermal analysis (DMTA), respectively. In theory, evidenced that the chemical grafting of CNW enhances their compatibility with the polymeric matrix and thus improves the final properties of the nanocomposites. Large modification of the crystalline properties such as the crystallization half-time was evidenced according to the nature of the PLA matrix and the content of nanofillers.

Keywords: cellulose nanowhiskers, nanocomposites, coconut husk fiber, ring opening polymerization

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Authors: Z. Miao, Y. Chu, Y. Zhang

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The unique cholesteric phase liquid crystals obtained by mixing nematic liquid crystals with chiral dopants have gained valuable applications in the display field for their selective reflection and circular dichroism properties. The periodic arrangement of the helical structure of cholesteric liquid crystals makes it possible to produce Bragg reflection of circularly polarized light irradiated perpendicularly to the liquid crystals and, therefore, to acquire semi- or fully reflective surfaces or films. If the polymer-liquid crystal composites are combined with polymeric monomers, commercialized reflective broadband films can be fabricated. In this study, the polymer-liquid crystal composites reflecting visible light region (wavelength centered at 550 nm) were studied to analyze the effects of AC electric field at different voltages and frequencies on the optical texture of the composites, as well as the effects of polymerization temperature and ultraviolet (UV) intensity on the polymerization reaction and reflection bandwidth. The optimal sample was finally obtained at 100Hz, 120V, 30℃, 1.00 mW/cm², which provides a research suggestion to solve the influencing factors of visible light reflection bandwidths.

Keywords: cholesteric liquid crystal, reflection bandwidths, negative dielectric anisotropy, planar texture

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Authors: Tasnuva Tamanna, Aimin Yu

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Application of nanoscience in biomedical field has come across as a new era. This study involves the synthesis of nano drug carrier with antibiotic loading. Based on the founding that polydopamine (PDA) nanoparticles could be formed via self-polymerization of dopamine at alkaline pH, one-step synthesis of rifampicin coupled polydopamine (PDA-R) nanoparticles was achieved by adding rifampicin into the dopamine solution. The successful yield of PDA nanoparticles with or without the presence of rifampicin during the polymerization process was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy. Drug loading was monitored by UV-vis spectroscopy and the loading efficiency of rifampicin was calculated to be 76%. Such highly capacious nano-reservoir was found very stable with little drug leakage at pH 3.

Keywords: drug loading, nanoparticles, polydopamine, rifampicin

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Authors: R. Saint-Loup, H. Amedro, N. Jacquel, S. Legrand, F. Fenouillot, J. P. Pascault, A. Rousseau

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Isosorbide or 1,4-3,6 dianhydrohexitol has been developped for several years as a new biobased monomer. It is commercially available as a starch derivative, more precisely obtained derivated from starch and more precisely from sorbitol. Isosorbide can find several applications, directly as a monomer or after chemical modification, in different polymer fields like thermoplastics (obtained from polycondensation or from radical polymerization of unsaturated monomers) or like Thermosetting resins (like cross linked PU, or after modification like acrylates or epoxy coatings) Concerning aliphatic or semi-aromatic polyesters, the addition of isosorbide improves thermal stability an,d optical properties, allowing a large range of applications as semi-crystalline or amorphous polymers. The preparation of poly (ethylene-co-isosorbide) terephthalate with different ratios of isosorbide will be particularly detailed. The structure – properties relationship will permit a focus on the obtention of polyesters with semi-crystalline or amorphous structures. The influence of isosorbide on the polymerization, on the processing of the resulting polyester as well as the modification of the final properties will be enlightened. The properties of Poly (ethylene-co-isosorbide) terephthlate will be emphasized and related to their applications. The evolutions related to Isosorbide with the replacement of ethylene glycol by Cyclohexanedimethanol allowed to drastically change the properties of the resulting polyester, with a large gap on the properties and new potential applications.

Keywords: modified PET, poly(ethylene-co-isosorbide)terephthalate, specialy polyester, poly(isosorbide_co_cyclohexanediol)terephthalate

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Authors: Woledegebrieal Aregay

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Introduction: Family planning is defined as the ability of individuals and couples to anticipate and attain their desired number of children and the spacing and timing of their births. It is part of a strategy to reduce poverty, maternal, infant and child mortality; empowers women by lightening the burden of excessive childbearing. Family planning is achieved through the use of different contraceptive methods among which the most effective method is modern family planning methods like Long-Acting Reversible Contraceptive (LARCs) which are IUCD and Implant and these methods have multiple advantages over other reversible methods. Most importantly, once in place, they do not require maintenance and their duration of action is long, ranging from 3 to10 years. Methods: An institutional-based cross-sectional study was conducted in Gondar town among female college students from April-May. A simple random sampling technique was employed to recruit a total of 1166 study subjects. Descriptive variables were computed for all predictors & dependent variables. The presence of an association between covariates & LARC use was observed by two tables’ findings using the chi-square test. Bivariate logistic regression was conducted to identify all possible factors affecting LARC utilization & its crude Odds Ratio, 95% Confidence Interval (CI) & P-value was observed. A multivariable logistic regression model was developed to control possible confounding variables. Adjusted Odds Ratio (AOR) with 95% Confidence Interval (CI) &P-values will be computed to identify significantly associated factors (P < 0.05) with LARC utilization. Result: Utilization of LARCs was 20.4%, the most common is Implant 86(96.5%), and followed by Intra-Uterine Contraceptive Device (IUCD) 3(3.5%). The result of the multivariate analysis revealed that the significant association of marital status of the respondent on utilization of LARC [AOR 3.965(2.051-7.665)], discussion of the respondent about LARC utilization with the husband/boyfriend [AOR 2.198(1.191-4.058)], and attitude of the respondent on implant was found to be associated [AOR 0.365(0.143-0.933)].Conclusion: The level of knowledge and attitude in this study was not satisfactory, the utilization of long-acting reversible contraceptives among college students was relatively satisfactory but if the knowledge and attitude of the participant has improved the prevalence of LARC were increased.

Keywords: utilization, long-acting reversible contraceptive, Ethiopia, Gondar

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Authors: K. M. Salim Reza, M. Hafiz Mia, M. A. Aziz, M. A. Motin, M. M. Rahman, M. A. Hasem

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The redox behavior of Fe (III) in presence of Catechol (Cc) has been carried out in buffer solution of different pH, scan rate, variation of Fe (III) concentration and Cc concentration. Uncoordinated Fe(III) or Cc has been found to undergo reversible electrode reaction whereas coordinated Fe-Cc is irreversible. The peak positions of the voltammogram of Fe- Cc shifted with respect to that of free Fe (III) or Cc and also developed a new peak at 0.12 V. The peak current of Fe-Cc decreases significantly compared with that of free Fe(III) or Cc in the same experimental conditions. These behaviors ascribed the formation of complex of Fe with Cc. The complex was formed either by the addition of Cc into Fe(III) or by the addition of Fe(III) into Cc. The effect of pH of Fe-Cc complex was studied by varying pH from 2 to 8.5. The electro chemical oxidation of Fe-Cc is facilitated in lower pH media. The slope of the plots of anodic peak current, Ep against pH of Fe-Cc complexe is 30 mV, indicates that the oxidation of Fe-Cc complexes proceeded via the 2e−/2H+ processes. The proportionality of the anodic and cathodic peak currents with square root of scan rate of suggests that the peak current of the different complexes at each redox reaction is controlled by diffusion process.

Keywords: cyclic voltammetry, Fe-Cc Complex, pH effect, redox interaction

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Authors: Thirawudh Pongprayoon, Watcharin Rassamee

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Silica-filled natural rubber compounds were prepared from unmodified and surface-modified silica. The modified silica was coated by ultrathin film of polyisoprene by admicellar polymerization. FTIR and SEM were applied to characterize the modified silica. The cure, mechanic, and dynamics properties were investigated with the comparison of the compounds. Cure characterization of modified silica rubber compound was shorter than that of unmodified silica compound. Strength and abrasion resistance of modified silica compound were better than those of unmodified silica rubber compound. Wet grip and rolling resistance analyzed by DMA from tanδ at 0°C and 60°C using 5 Hz were also better than those of unmodified silica rubber compound.

Keywords: silica, admicellar polymerization, rubber compounds, mechanical properties, dynamic properties

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Authors: Marcin Zieliński, Marcin Dębowski, Mirosław Krzemieniewski

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This publication presents a device designed for mechanical fragmentation of plant substrate before methane fermentation. The device is equipped with a perforated rotary cylindrical drum coated with a thermal layer, connected to a substrate feeder and driven by a motoreducer. The drum contains ball- or cylinder-shaped weights of different diameters, while its interior is mounted with lateral permanent magnets with an attractive force ranging from 100 kg to 2 tonnes per m2 of the surface. Over the perforated rotary drum, an infrared radiation generator is mounted, producing 0.2 kW to 1 kW of infrared radiation per 1 m2 of the perforated drum surface. This design reduces the energy consumption required for the biomass destruction process by 10-30% in comparison to the conventional ball mill. The magnetic field generated by the permanent magnets situated within the perforated rotary drum promotes this process through generation of free radicals that act as powerful oxidants, accelerating the decomposition rate. Plant substrate shows increased susceptibility to biodegradation when subjected to magnetic conditioning, reducing the time required for biomethanation by 25%. Additionally, the electromagnetic radiation generated by the radiator improves substrate destruction by 10% and the efficiency of the process. The magnetic field and the infrared radiation contribute synergically to the increased efficiency of destruction and conversion of the substrate.

Keywords: biomass pretreatment, mechanical fragmentation, biomass, methane fermentation

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Authors: M. N. Abu Seman, L. M. Kei, M. A. Yusoff

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Forward Osmosis (FO) polyamide thin-film composite membranes have been prepared by inter facial polymerization using commercial UF polyethersulfone as membrane support. Different inter facial polymerization times (10s, 30s and 60s) in the organic solution containing trimesoyl chloride (TMC) at constant m-phenylenediamine (MPD) concentration (2% w/v) were studied. The synthesized polyamide membranes then tested for treatment of natural organic matter (NOM) and compared to commercial Cellulose TriAcetate (CTA) membrane. It was found that membrane prepared with higher reaction time (30 s and 60 s) exhibited better membrane performance (flux and humic acid removal) over commercial CTA membrane.

Keywords: cellulose triacetate, forward osmosis, humic acid, polyamide

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Authors: Michael A. Kraus, Navid Pourmoghaddam, Martin Botz, Jens Schneider, Geralt Siebert

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Fragmentation analysis of tempered glass gives insight into the quality of the tempering process and defines a certain degree of safety as well. Different standard such as the European EN 12150-1 or the American ASTM C 1048/CPSC 16 CFR 1201 define a minimum number of fragments required for soda-lime safety glass on the basis of fragmentation test results for classification. This work presents an approach for the glass breakage pattern prediction using a Voronoi Tesselation over Random Fields. The random Voronoi tessellation is trained with and validated against data from several breakage patterns. The fragments in observation areas of 50 mm x 50 mm were used for training and validation. All glass specimen used in this study were commercially available soda-lime glasses at three different thicknesses levels of 4 mm, 8 mm and 12 mm. The results of this work form a Bayesian framework for the training and prediction of breakage patterns of tempered soda-lime glass using a Voronoi Random Field Tesselation. Uncertainties occurring in this process can be well quantified, and several statistical measures of the pattern can be preservation with this method. Within this work it was found, that different Random Fields as basis for the Voronoi Tesselation lead to differently well fitted statistical properties of the glass breakage patterns. As the methodology is derived and kept general, the framework could be also applied to other random tesselations and crack pattern modelling purposes.

Keywords: glass breakage predicition, Voronoi Random Field Tessellation, fragmentation analysis, Bayesian parameter identification

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Authors: M. Cabuk, M. Yavuz, T. A. Yesil, H. I. Unal

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Electrorheological (ER) fluids are a class of smart materials exhibiting reversible changes in their rheological and mechanical properties under an applied electric field (E). ER fluids generally are composed of polarisable solid particles dispersed in non-conducting oil. ER fluids are fluids which exhibit. The resistance to motion of the ER fluid can be controlled by adjusting the applied E, due to their fast and reversible changes in their rheological properties presence of E. In this study, a series of chitosan/expanded perlite (CS/EP) composites with different chitosan mass fractions (10%, 20%, and 50%) was used. Characterizations of the composites were carried out by Fourier Transform Infrared (FTIR), X-ray diffraction (XRD) and Scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX) techniques. Antisedimentation stability and dielectric properties of the composites were also determined. The effects of volume fraction, electric field strength, shear rate, shear stress, and temperature onto ER properties of the CS/EP composite particles dispersed in silicone oil (SO) were investigated in detail. Vibration damping behavior of the CS/EP composites were determined as a function of frequence, storage (Gʹ) and loss (Gʹ ʹ) moduli. It was observed that ER response of the CS/EP/SO ER fluids increased with increasing electric field strength and exhibited the typical shear thinning non-Newtonian viscoelastic behaviors with increasing shear rate. The maximum yield stress was obtained with 1250 Pa under E = 3 kV/mm. Further, the CS/EP/SO ER fluids were observed to sensitive to vibration control by showing reversible viscosity enhancements (Gʹ > Gʹ ʹ). Acknowledgements: The authors thank the TÜBİTAK (214Z199) for the financial support of this work.

Keywords: chitosan, electrorheology, perlite, vibration control

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Authors: Yaseen Elhebshi, Abdulkareem Hamid, Nureddin Bin Issa, Xiaonong Chen

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A convenient method of preparing ultrafine polystyrene latex nano-particles with amino groups on the surface is developed. Polystyrene latexes in the size range 50–400 nm were prepared via emulsion polymerization, using sodium dodecyl sulfate (SDS) as surfactant. Polystyrene with amino groups on the surface will be fine to use as organic filler to modify rubber. Transmission electron microscopy (TEM) was used to observe the morphology of silicon dioxide and functionalized polystyrene nano-particles. The nature of bonding between the polymer and the reactive groups on the filler surfaces was analyzed using Fourier transform infrared spectroscopy (FTIR). Scanning electron microscopy (SEM) was employed to examine the filler surface.

Keywords: reactive filler, emulsion polymerization, particle size, polystyrene nanoparticles

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Authors: Magdi. M. Nabi, Ding-Li Yu

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Control of a semi-batch polymerization reactor using an adaptive radial basis function (RBF) neural network method is investigated in this paper. A neural network inverse model is used to estimate the valve position of the reactor; this method can identify the controlled system with the RBF neural network identifier. The weights of the adaptive PID controller are timely adjusted based on the identification of the plant and self-learning capability of RBFNN. A PID controller is used in the feedback control to regulate the actual temperature by compensating the neural network inverse model output. Simulation results show that the proposed control has strong adaptability, robustness and satisfactory control performance and the nonlinear system is achieved.

Keywords: Chylla-Haase polymerization reactor, RBF neural networks, feed-forward, feedback control

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Authors: Ipek Gunay, Efe B. Orman, Metin Ozer, Bekir Salih, Ali R. Ozkaya

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Phthalocyanines with macrocyclic ring containing at least three heteroatoms have nine or more membered structures. Metal-free phthalocyanines react with metal salts to obtain chelate complexes. This is one of the most important features of metal-free phthalocyanine as ligand structure. Although phthalocyanines have very similar properties with porphyrins, they have some advantages such as lower cost, easy to prepare, and chemical and thermal stability. It’s known that Pc compounds have shown one-electron metal-and/or ligand-based reversible or quasi-reversible reduction and oxidation processes. The redox properties of phthalocyanines are critically related to the desirable properties of these compounds in their technological applications. Thus, Pc complexes have also been receiving increasing interest in the area of fuel cells due to their high electrocatalytic activity in dioxygen reduction and fuel cell applications. In this study, novel phthalocyanine complexes coordinated with Fe(II) and Co (II) to be used as catalyst were synthesized. Aiming this goal, a new nitrile ligand was synthesized starting from 4-hydroxy-3,5-dimethoxy benzyl alcohol and 4-nitrophthalonitrile in the presence of K2CO3 as catalyst. After the isolation of the new type of nitrile and metal complexes, the characterization of mentioned compounds was achieved by IR, H-NMR and UV-vis methods. In addition, the electrochemical behaviour of Pc complexes was identified by cyclic voltammetry, square wave voltammetry and in situ spectroelectrochemical measurements. Furthermore, the catalytic performances of Pc complexes for oxygen reduction were tested by dynamic voltammetry measurements, carried out by the combined system of rotating ring-disk electrode and potentiostat, in a medium similar to fuel-cell working conditions.

Keywords: phthalocyanine, electrocatalysis, electrochemistry, in-situ spectroelectrochemistry

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Authors: A. Douka, S. Vouyiouka, L. M. Papaspyridi, D. Korres, C. Papaspyrides

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A "green" process was studied for the preparation of partially renewable aliphatic polyesters based on 1,4-butanediol and 1,8-octanediol with various diacids and derivatives, namely diethyl succinate, adipic acid, sebacic acid, 1,12-dodecanedioic acid and 1,14-tetradecanedioic acid. A first step of enzymatic prepolymerization was carried out in the presence of two different solvents, toluene and diphenylether, applying molecular sieves and vacuum, respectively, to remove polycondensation by-products. Poly(octylene adipate) (PE 8.6), poly(octylene dodecanate)(PE 8.12) and poly(octylene tetradecanate) (PE 8.14) were firstly enzymatically produced in toluene using molecular sieves giving however, low-molecular-weight products. Thereafter, the synthesis of PE 8.12 and PE 8.14 was examined under optimized conditions using diphenylether as solvent and a more vigorous by-product removal step, such as application of vacuum. Apart from these polyesters, the optimized process was also implemented for the production of another long-chain polyester-poly(octylene sebacate) (PE 8.10) and a short-chain polyester-poly(butylene succinate) (PE 4.4). Subsequently, bulk post-polymerization in the melt or solid state was performed. SSP runs involved absence of biocatalyst and reaction temperatures (T) in the vicinity of the prepolymer melting point (Tm-T varied between 15.5 up to 4oC). Focusing on PE 4.4 and PE 8.12, SSP took place under vacuum or flowing nitrogen leading to increase of the molecular weight and improvement of the end product physical appearance and thermal properties.

Keywords: aliphatic polyester, enzymatic polymerization, solid state polymerization, Novozym 435

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Authors: Angelo Lanzilotto, Martin Kuss-Petermann, Catherine E. Housecroft, Edwin C. Constable, Oliver S. Wenger

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We recently described the synthesis of a new tetraphenylporphyrinatozinc(II)-conjugated 2,2':6',6"-terpyridine (1) in which the tpy domain enables the molecule to act as a metalloligand. The synthetic route to 1 has been optimized, the importance of selecting a particular sequence of synthetic steps will be discussed. Three homoleptic complexes have been prepared, [Zn(1)₂]²⁺, [Fe(1)₂]²⁺ and [Ru(1)₂]²⁺, and have been isolated as the hexafluoridophosphate salts. Spectroelectrochemical measurements have been performed and the spectral changes ascribed to redox processes are partitioned on either the porphyrin or the terpyridine units. Compound 1 undergoes a reversible one-electron oxidation/reduction. The removal/gain of a second electron leads to a further irreversible chemical transformation. For the homoleptic [M(1)₂]²⁺ complexes, a suitable potential can be chosen at which both the oxidation and the reduction of the {ZnTPP} core are reversible. When the homoleptic complex contains a redox active metal such as Fe or Ru, spectroelectrochemistry has been used to investigate the metal to ligand charge transfer (MLCT) transition. The latter is sensitive to the oxidation state of the metal, and electrochemical oxidation of the metal center suppresses it. Detailed spectroelectrochemical studies will be presented.

Keywords: homoleptic complexes, spectroelectrochemistry, tetraphenylporphyrinatozinc(II), 2, 2':6', 6"-terpyridine

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Authors: Hu-Cheng Weng, Jhen-Ting Huang, Chia-Chia Chang, An-Ya Lo

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In this study, carbon mesoporous material, CMK-3, was adopted as supporting material for electroactive polymerspolyaniline (PANI), polyaniline, for supercapacitor application, where hydroquinone (HQ) was integrated to enhance the redox reaction of PANI. The results show that the addition of PANI improves the capacitance of electrode from 89 F/g (CMK-3) to 337 F/g (PANI/CMK-3), the addition of HQ furtherly improves the capacitance to 463 F/g (PANI/CMK-3/HQ). The PANI provides higher energy density and also acts as binder of the electrode; the CMK-3 provides higher electron double layer capacitance EDLC and stabilize the polyaniline by its highly porosity. With the addition of HQ, the capacitance of PANI/CMK-3 was further enhanced. In-situ analyses including cyclic voltammetry (CV), chronopotentiometry (CP), electron impedance spectrum (EIS) analyses were applied for electrode performance examination. For materials characterization, the crystal structure, morphology, microstructure, and porosity were examined by X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscopy (TEM), and 77K N2 adsorption/desorption analyses, respectively. The effects of electrolyte pH value, PANI polymerization time, HQ concentration, and PANI/CMK-3 ratio on capacitance were discussed. The durability was also studied by long-term operation test. The results show that PANI/CMK-3/HQ with great potential for supercapacitor application. Finally, the potential of all-solid PANI/CMK-3/HQ based supercapacitor was successfully demonstrated.

Keywords: CMK3, PANI, redox electrolyte, solid supercapacitor

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Authors: Nagi Greesh

Abstract:

This study highlights a new method to obtain multiphase composites particles containing hydrophobic (wax) and inorganic (clay) compounds. Multiphase polystyrene-clay-wax nanocomposites were successfully synthesized. Styrene monomer were polymerized in the presence of different wax-clay nanocomposites concentrations in miniemulsion. Wax-clay nanocomposites were firstly obtained through ultrasonic mixing at a temperature above the melting point of the wax at different clay loadings. The obtained wax-clay nanocomposites were then used as filler in the preparation of polystyrene-wax-clay nanocomposites via miniemulsion polymerization. The particles morphology of PS/wax-clay nanocomposites latexes was mainly determined by Transmission Electron Microscopy ( TEM) , core/shell morphology was clearly observed, with the encapsulation of most wax-clay nanocomposites inside the PS particles. On the other hand, the morphology of the PS/wax-clay nanocomposites (after film formation) ranged from exfoliated to intercalated structures, depending on the percentage of wax-clay nanocomposites loading. This strategy will allow the preparation materials with tailored properties for specific applications such as paint coatings and adhesives.

Keywords: polymer-wax, paraffin wax, miniemulsion, core/shell, nanocomposites

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Authors: Sutar Rani Ananda, M. V. Murugendrappa

Abstract:

To investigate electrical properties of conducting polypyrrole (PPy) and cobalt aluminum oxide (CAO) nanocomposites, impedance analyzer in frequency range of 100 Hz to 5 MHz is used. In this work, PPy/CAO nanocomposites were synthesized by chemical oxidation polymerization method in different weight percent of CAO in PPy. The dielectric properties and AC conductivity studies were carried out for different nanocomposites in temperature range of room temperature to 180 °C. With the increase in frequency, the dielectric constant for all the nanocomposites was observed to decrease. AC conductivity of PPy was improved by addition of CAO nanopowder.

Keywords: polypyrrole, dielectric constant, dielectric loss, AC conductivity

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Authors: H. E. M. W. G. M. K. Ekanayake, J. Dharmasena

Abstract:

Natural Landscape fragmentation and habitat loss are emerging issues in Sri Lanka, which is due to rapid urban development and inadequate concern of managing Landscape connectivity. Urban Wetlands are the most vulnerable ecosystem effects from the fragmentation. Therefore, management of landscape connectivity with proper analysis and understanding has become a most important measure for urban wetland habitats. This study aimed to introduce spatial planning strategy to identify and locate landscape developments appropriately in order to restore landscape connectivity. Therefore, the study focuses on understanding the relationship between habitat patch metrics and landscape connectivity with reference to Colombo wetlands. Geographic Information Systems (GIS) was used to measure the wetland patch metrics; Patch area, Total edge, Perimeter-area ratio, Core area index and Inter-patch distances. Further, GIS-enabled least-cost path tool was used to measure the Landscape connectivity and calculate the number of species flow paths per wetland patch. According to the research findings; increasing the patch area, maintaining a mean perimeter-area ratio and core area index also reducing the inter-patch distances could enhance the landscape connectivity. Further, this study introduces three patch typologies; ‘active patches,' ‘open patches’ and ‘closed patches’ that severs to landscape connectivity in different levels. In the end, the study proposes a strategy for Landscape Architects to select most suitable locations to implement ecological based landscape developments with adjacent to the existing urban habitat in order to enhance habitat patch metrics and to restore the landscape connectivity.

Keywords: landscape fragmentation, urban wetlands, landscape connectivity, patch metrics

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Authors: Guillaume Soubeyran, Fabrice Micoud, Benoit Morin, Jean-Philippe Poirot-Crouvezier, Magali Reytier

Abstract:

Proton Exchange Membrane Fuel Cell (PEMFC) technology is considered as a solution for the reduction of CO2 emissions. However, this technology still meets several challenges for high-scale industrialization. In this context, the increase of durability remains a critical aspect for competitiveness of this technology. Fortunately, performance degradations in nominal operating conditions is partially reversible, meaning that if specific conditions are applied, a partial recovery of fuel cell performance can be achieved, while irreversible degradations can only be mitigated. Thus, it is worth studying the optimal conditions to rejuvenate these reversible degradations and assessing the long-term impact of such procedures on the performance of the cell. Reversible degradations consist mainly of anode Pt active sites poisoning by carbon monoxide at the anode, heterogeneities in water management during use, and oxidation/deactivation of Pt active sites at the cathode. The latter is identified as a major source of reversible performance loss caused by the presence oxygen, high temperature and high cathode potential that favor platinum oxidation, especially in high efficiency operating points. Hence, we studied here a recovery procedure aiming at reducing the platinum oxides by decreasing cathode potential during operation. Indeed, the application of short air starvation phase leads to a drop of cathode potential. Cell performances are temporarily increased afterwards. Nevertheless, local temperature and current heterogeneities within the cells are favored and shall be minimized. The consumption of fuel during the recovery phase shall also be considered to evaluate the global efficiency. Consequently, the purpose of this work is to find an optimal compromise between the recovery of reversible degradations by air starvation, the increase of global cell efficiency and the mitigation of irreversible degradations effects. Different operating parameters have first been studied such as cell voltage, temperature and humidity in single cell set-up. Considering the global PEMFC system efficiency, tests showed that reducing duration of recovery phase and reducing cell voltage was the key to ensure an efficient recovery. Recovery phase frequency was a major factor as well. A specific method was established to find the optimal frequency depending on the duration and voltage of the recovery phase. Then, long-term degradations have also been studied by applying FC-DLC cycles based on NEDC cycles on a 4-cell short stack by alternating test sequences with and without recovery phases. Depending on recovery phase timing, cell efficiency during the cycle was increased up to 2% thanks to a mean voltage increase of 10 mV during test sequences with recovery phases. However, cyclic voltammetry tests results suggest that the implementation of recovery phases causes an acceleration of the decrease of platinum active areas that could be due to the high potential variations applied to the cathode electrode during operation.

Keywords: durability, PEMFC, recovery procedure, reversible degradation

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Authors: Sasan Talebnezhad, Saeed Pormahdian, Naghi Assali

Abstract:

Homogeneous α-diimine nickel (II) catalyst complexes, with and without amino para-aryl position functionality, were synthesized. These complexes were immobilized on carboxyl, hydroxyl, and acyl chloride functionalized multi-walled carbon nanotubes to form five novel heterogeneous α-diiminonickel catalysts. Immobilization was performed by covalent or electrostatic bonding via methylaluminoxane (MAO) linker or amide linkage. Both the nature of α-diimine ligands and the kind of interaction between anchored catalyst complexes and multi-walled carbon nanotube surface influenced the catalytic performance, microstructure, and morphology of obtained polyethylenes. The catalyst prepared by amide bonding showed lowest relative weight loss in thermogravimetry analysis and highest activities up to 5863 gr PE mmol-1Ni.hr-1. This catalyst produced polyethylene with dense botryoidal morphology.

Keywords: α-diimine nickel (II) complexes, immobilization, multi-walled carbon nanotubes, ethylene polymerization

Procedia PDF Downloads 385

Authors: Sasan Talebnezhad, Saeed Pourmahdian, Naghi Assali

Abstract:

Homogeneous α-diimine nickel (II) catalyst complexes, with and without amino para-aryl position functionality, were synthesized. These complexes were immobilized on carboxyl, hydroxyl and acyl chloride functionalized multi-walled carbon nanotubes to form five novel heterogeneous α diiminonickel catalysts. Immobilization was performed by covalent or electrostatic bonding via methylaluminoxane (MAO) linker or amide linkage. Both the nature of α-diimine ligands and the kind of interaction between anchored catalyst complexes and multi-walled carbon nanotube surface influenced the catalytic performance, microstructure, and morphology of obtained polyethylenes. The catalyst prepared by amide bonding showed lowest relative weight loss in thermogravimetry analysis and highest activities up to 5863 gr PE mmol-1Ni.hr-1. This catalyst produced polyethylene with dense botryoidal morphology.

Keywords: α-diimine nickel (II) complexes, immobilization, multi-walled carbon nanotubes, ethylene polymerization

Procedia PDF Downloads 476