Ultrasound assisted preparation, characterization and adsorption study of ternary chitosan-ZnO-TiO2 nanocomposite: Advantage over conventional method.

In the present work, the synthesis of ternary chitosan/zinc oxide/titanium dioxide (CTS-ZnO-TiO2) nanocomposite was carried out with the use of mechanical stirring (conventional) and ultrasound assisted method. The characterization of prepared CTS-ZnO-TiO2 adsorbent was carried out using XRD, TEM, FTIR and the results of these analysis methods proved the successful preparation of ternary nanocomposite. Crystal violet (CV) dye was used as a pollutant to observe the adsorption ability of the prepared nanocomposite and the nanocomposite prepared by ultrasonic-assisted method proved to be a better adsorbent. The CV dye adsorption was significant for CTS-ZnO-TiO2 nanocomposite synthesized with the use of ultrasound assisted method compared to that prepared by conventional method. It is due to the physical effects of the ultrasonic irradiations due to which formation of finely dispersed nanocomposite takes place than that by conventional method. For batch adsorption the effect of various operating parameters such as initial dye concentration, time, temperature and adsorbent dose has been evaluated. The obtained data were processed using isotherm models, adsorption kinetics and the thermodynamic behavior of the cationic dye adsorption was also studied. The isotherm data was correlated reasonably well by the Temkin adsorption isotherm. Pseudo-second-order kinetic model provided a better correlation for the experimental data compared to pseudo first order, Elovich model and power function kinetics model. Thermodynamic parameters for adsorption indicated that the dye adsorption was spontaneous and endothermic in nature.

Ultrasound effects based on simulation of milk processing properties.

Efficient reconstitution followed by fermentation of nonfat (skimmed) dry milk is one of the most important aspects in manufacturing of various dairy products. As a first stage, dry milk is normally being reconstituted using conventional approaches such as heating and stirring the mixture. Nevertheless, we demonstrated, that low-frequency (22 ±â€¯1.65 kHz) ultrasound can be used as an alternative to the traditional methods of milk recovery. Low-frequency ultrasound was applied during pre-fermentation stage to improve the dispersity of the resulting milk product and to create good conditions for a post-ultrasound bacterial fermentation of milk. The applied ultrasound power was set in the range of 60-120 W/L. For the fermentation process we used: kefir fungi, fermenter of direct inoculation for yogurt LYOBAC YOYO and mixed culture for kefir LAT LC K. The effectiveness of ultrasound treatment was evaluated based on the accumulation of exopolysaccharides (EPS), vitamin C content, as well as antioxidant activity of the resulting milk product. The effect of ultrasound on microflora and the role of the specific types of bacteria such as Lactobacillus on the accumulation of biologically active compounds in the fermented milk products was studied with use of electron microscopy and MALDI - to FMS method. Overall, our results showed that reconstitution of dry milk with use of ultrasound improves further accumulation of biologically active compounds and rises the nutritional quality of the fermented product.

Sonochemical synthesis of Graphene-Ce-TiO2 and Graphene-Fe-TiO2 ternary hybrid photocatalyst nanocomposite and its application in degradation of crystal violet dye.

The present work deals with the preparation of graphene oxide (GO) using Hummers-Offeman method in the presence of ultrasonic irradiations. Further loading of TiO2 photocatalyst on prepared GO was accomplished which is basically oxidation reduction reaction between graphene oxide and titanium isopropoxide that leads to the formation of graphene-TiO2 nanocomposite. Graphene-Ce-TiO2 and Graphene-Fe-TiO2 nanocomposites were prepared using one step in-situ ultrasound assisted method using GO, titanium isopropoxide, cerium nitrate, ferric nitrate, and 2-propanol. The successfully prepared graphene-TiO2, Graphene-Ce-TiO2, Graphene-Fe-TiO2 nanocomposites were then characterized using XRD, SEM and TEM analysis. The obtained XRD patterns clearly indicates the formation of anatase TiO2 on graphene nanosheets and it also indicates the presence of Ce and Fe in the Graphene-Ce-TiO2 and Graphene-Fe-TiO2 nanocomposite respectively. Further the use of the prepared nanocomposites as a photocatalyst have been studied for the degradation of crystal violet dye. The effect of various parameters such as catalyst doping, catalyst loading and initial concentration of dye on its degradation were studied. The effectiveness of the prepared catalysts were compared for the degradation of crystal violet dye. It has been observed that Graphene-Fe-TiO2 exhibits maximum photocatalytic activity compared to Graphene-Ce-TiO2 and Graphene-TiO2 nanocomposite photocatalyst.

Ultrasound assisted synthesis of performic acid in a continuous flow microstructured reactor.

The present work establishes in depth study of ultrasound assisted preparation of performic acid (PFA) in a continuous flow microstructured reactor. The influence of various parameters viz. formic acid: hydrogen peroxide molar ratio, flow rate, temperature and catalyst loading on the PFA formation were studied in a continuous flow microstructured reactor. In a continuous microstructured reactor in the presence of ultrasonic irradiation, the formation of PFA was found to be dependent on the molar ratio of formic acid: hydrogen peroxide, flow rate of reactants, temperature and catalyst loading (Amberlite IR-120H). The optimized parameter values are 1:1M ratio, 50mL/h, 40°C and 471mg/cm3 respectively. Further, the performance of Amberlite IR-120H catalyst was evaluated for three successive cycles in continuous microstructured reactor. The performance of catalyst was found to be decreased with the usage of the catalyst and is attributed to neutralization of the sulfonic acid groups, catalyst shrinkage, or loss in pore sites. The experimental results revealed that, for an ultrasound assisted synthesis of PFA in continuous microstructured reactor the observed reaction time was even less than 10min. The observed intensification in the PFA synthesis process can be attributed to the intense collapse of the cavities formed at low temperature during ultrasonic irradiations, which further improved the heat and mass transfer rates with the formation of H2O2 during the reaction. The combined use of ultrasound and a continuous flow microstructured reactor has proved beneficial process of performic acid synthesis.

Intensification of extraction of curcumin from Curcuma amada using ultrasound assisted approach: Effect of different operating parameters.

Curcumin, a dietary phytochemical, has been extracted from rhizomes of Curcuma amada using ultrasound assisted extraction (UAE) and the results compared with the conventional extraction approach to establish the process intensification benefits. The effect of operating parameters such as type of solvent, extraction time, extraction temperature, solid to solvent ratio, particle size and ultrasonic power on the extraction yield have been investigated in details for the approach UAE. The maximum extraction yield as 72% was obtained in 1h under optimized conditions of 35°C temperature, solid to solvent ratio of 1:25, particle size of 0.09mm, ultrasonic power of 250W and ultrasound frequency of 22kHz with ethanol as the solvent. The obtained yield was significantly higher as compared to the batch extraction where only about 62% yield was achieved in 8h of treatment. Peleg's model was used to describe the kinetics of UAE and the model showed a good agreement with the experimental results. Overall, ultrasound has been established to be a green process for extraction of curcumin with benefits of reduction in time as compared to batch extraction and the operating temperature as compared to Soxhlet extraction.

Improved synthesis of aluminium nanoparticles using ultrasound assisted approach and subsequent dispersion studies in di-octyl adipate.

The present work reports on an efficient and simple one pot synthetic approach for aluminium nanoflakes and nanoparticles based on the intensification using ultrasound and provides a comparison with the conventional approach to establish the cutting edge process benefits. In situ passivation of aluminium particles with oleic acid was used as the method of synthesis in both the conventional and ultrasound assisted approaches. The aluminium nanoflakes prepared using the ultrasound assisted approach were subsequently dispersed in di-octyl adipate (DOA) and it was demonstrated that a stable dispersion of aluminium nanoflakes into di-octyl adipate (DOA) is achieved. The morphology of the synthesized material was established using the transmission electron microscopy (TEM) analysis and energy dispersive X-ray analysis (EDX) and the obtained results confirmed the metal state and nano size range of the obtained aluminium nanoflakes and particles. The stability of the aluminium nanoflakes obtained using ultrasound assisted approach and nanoparticles using conventional approach were characterized using the zeta potential analysis and the obtained values were in the range of -50 to +50mV and -100 to +30mV respectively. The obtained samples from both the approaches were also characterized using X-ray diffraction (XRD) and particle size analysis (PSA) to establish the crystallite size and particle distribution. It was observed that the particle size of the aluminium nanoflakes obtained using ultrasound assisted approach was in the range of 7-11nm whereas the size of aluminium nanoparticles obtained using conventional approach was much higher in the range of 1000-3000nm. Overall it was demonstrated that the aluminium nanoflakes obtained using the ultrasound assisted approach showed excellent morphological characteristics and dispersion stability in DOA showing promise for the high energy applications.

A novel approach for continuous synthesis of calcium carbonate using sequential operation of two sonochemical reactors.

A novel continuous process for the synthesis of calcium carbonate based on precipitation reaction has been developed involving the sequential operation of two sonochemical reactors for the first time. The reactors were also operated as control (conventional approach without ultrasound) to clearly establish the process intensification benefits due to the use of ultrasound. The effect of different operating parameters such as Ca(OH)2 concentration, CO2 flow rate and Ca(OH)2 slurry flow rate on the particle size has been investigated. The obtained calcite particles were characterized using Fourier transform infrared (FTIR), wide angle X-ray diffraction (XRD) and particle size distribution (PSD) analysis. The morphology of the obtained particles was also analyzed using scanning electron microscopy (SEM) and transmission electron microscopy (TEM). It was established that the average particle size obtained in the presence of ultrasound was smaller with much narrow size distribution as compared to the conventional approach. Further, the average particle size was established to decrease with an increase in the Ca(OH)2 slurry concentration and CO2 flow rate with the optimum conditions giving a particle size of 164nm. The particle size was also influenced by the Ca(OH)2 slurry flow rate and under optimum condition of Ca(OH)2 slurry flow rate as 24mL/min, particle size of 135nm was obtained. Only calcite phase of CaCO3 was observed to be formed as established based on the XRD analysis during both the synthesis approaches confirming the stability of the obtained particles. It was also observed that the shape of the crystals varied with the method of synthesis. Rhombohedral calcite particles were formed in the presence of ultrasound whereas the conventional stirring method resulted in spindle shaped particles. Overall, the utility of the ultrasound assisted approach has been clearly established with novel results based on the use of sonochemical reactors in series.

Investigation of TiO2 photocatalyst performance for decolorization in the presence of hydrodynamic cavitation as hybrid AOP.

In this article, an acoustic cavitation engineered novel approach for the synthesis of TiO2, cerium and Fe doped TiO2 nanophotocatalysts is reported. The prepared TiO2, cerium and Fe doped TiO2 nanophotocatalysts were characterized by XRD and TEM analysis to evaluate its structure and morphology. Photo catalytic performance of undoped TiO2 catalyst was investigated for the decolorization of crystal violet dye in aqueous solution at pH of 6.5 in the presence of hydro dynamic cavitation. Effect of catalyst doping with Fe and Ce was also studied for the decolorization of crystal violet dye. The results shows that, 0.8% of Fe-doped TiO2 exhibits maximum photocatalytic activity in the decolorization study of crystal violet dye due to the presence of Fe in the TiO2 and it may acts as a fenton reagent. Kinetic studies have also been reported for the hybrid AOP (HAOP) that followed the pseudo first-order reaction kinetics.

Intensification of ultrasound-assisted process for the preparation of spindle-shape sodium zinc molybdate nanoparticles.

In the present work, sodium zinc molybdate (SZM) nanoparticles were prepared using conventional and an innovative ultrasound assisted co-precipitation of sodium molybdate, zinc oxide and HNO3 at different temperatures. Prepared product was characterized by XRD, TEM, FT-IR, particle size distribution (PSD), TGA and DTA techniques. TEM analysis shows the spindle-shaped morphology of the formed SZM nanoparticles. The average particle size of SZM nanoparticles is found to be lower in case of sonochemical method (78.3 nm) compared to conventional method (340.2 nm) which is attributed to faster solute transfer rate due to ultrasonic irradiation leading to rapid nucleation and restricted growth of SZM nanoparticles. Further, the kinetics of synthesis of SZM nanoparticles are studied using the sonochemical method at different operating temperature and conventional method at 80°C. It is shown that the rate of reaction is significantly faster at 40°C compared to other temperatures and also conventional method. This can be attributed to intense cavity collapse at lower temperature (low vapour pressure) compared to higher temperature (high vapour pressure) of the reaction mixture.

Continuous precipitation of calcium carbonate using sonochemical reactor.

The continuous production of calcium carbonate (CaCO3) by precipitation method at room temperature was carried out in a stirred reactor under ultrasonic environment and was compared with the conventional stirring method. The effect of various operating parameters such as Ca(OH)2 slurry concentration, CO2 flow rate and Ca(OH)2 slurry flow rate on the particle size of CaCO3 was investigated. The calcium carbonate particles were characterized by Fourier transform infrared (FTIR), wide angle X-ray diffraction (WXRD) and particle size. The morphology was studied by using scanning electron microscopic (SEM) images. The particle size obtained in the presence of ultrasonic environment was found to be smaller as compared to conventional stirring method. The particle size is found to be reduced with an increase in the concentrations of Ca(OH)2 and increased with increasing CO2 flow rate for both the methods. The slurry flow rate had a major effect on the particle size and the particle size decreased with increased slurry flow rate. Only calcite phase of CaCO3 was predominantly present as confirmed by the characterization techniques for both the preparation methods. In most of the cases rhombohedral calcite particles were observed.

Ultrasound assisted synthesis of PANI/ZnMoO4 nanocomposite for simultaneous improvement in anticorrosion, physico-chemical properties and its application in gas sensing.

Ultrasound assisted in-situ semi-batch emulsion polymerization has been used for the preparation of polyaniline (PANI) and PANI/ZnMoO4 nanocomposite with different loading of ZnMoO4 (ZM) nanoparticles. ZM nanoparticles were functionalized using Myristic acid (MA) for better compatibility with PANI. The cavitational effects induced due to ultrasonic irradiations have been shown significant enhancement in the dispersion of functionalized ZM nanoparticles into the PANI during ultrasound assisted in-situ emulsion polymerization process. TEM images of PANI/ZM nanocomposite particles give the direct evidence of fine dispersion and encapsulation of MA treated ZM nanoparticles in PANI matrix. The presence of ZM nanoparticles in PANI/ZM nanocomposite shows significant improvement in the mechanical (cross-cut adhesion), thermal, anticorrosion and sensing properties of PANI/ZM nanocomposite/alkyd coatings over PANI/alkyd and neat alkyd resin coating. Fine and uniform dispersion of ZM nanoparticles in PANI matrix using this novel synthesis method (PANI (p-type)/ZM (n-type) hetero-junction) improves LPG sensing ability and minimizes response time to sense LPG significantly compared with neat PANI.

Ultrasound assisted synthesis of doped TiO2 nano-particles: characterization and comparison of effectiveness for photocatalytic oxidation of dyestuff effluent.

The present work deals with the synthesis of titanium dioxide nanoparticles doped with Fe and Ce using sonochemical approach and its comparison with the conventional doping method. The prepared samples have been characterized using X-ray diffraction (XRD), FTIR, transmission electron microscopy (TEM) and UV-visible spectra (UV-vis). The effectiveness of the synthesized catalyst for the photocatalytic degradation of crystal violet dye has also been investigated considering crystal violet degradation as the model reaction. It has been observed that the catalysts prepared by sonochemical method exhibit higher photocatalytic activity as compared to the catalysts prepared by the conventional methods. Also the Ce-doped TiO(2) exhibits maximum photocatalytic activity followed by Fe-doped TiO(2) and the least activity was observed for only TiO(2). The presence of Fe and Ce in the TiO(2) structure results in a significant absorption shift towards the visible region. Detailed investigations on the degradation indicated that an optimal dosage with 0.8 mol% doping of Ce and 1.2 mol% doping of Fe in TiO(2) results in higher extents of degradation. Kinetic studies also established that the photocatalytic degradation followed the pseudo first-order reaction kinetics. Overall it has been established that ultrasound assisted synthesis of doped photocatalyst significantly enhances the photocatalytic activity.

Production of cerium zinc molybdate nano pigment by innovative ultrasound assisted approach.

Ultrasound assisted synthesis of yellow rare earth cerium zinc molybdate anticorrosion nanopigment is presented. This new class of pigment is eco-friendly alternatives to lead, cadmium and chromium pigment as these pigments contains carcinogenic species like Cr(6+) which is responsible for human disease. The synthesis of nanosized cerium zinc molybdate was carried out using cerium nitrate, sodium zinc molybdate as a precursor materials by conventional and ultrasound assisted chemical precipitation method without addition of emulsification agent. XRD, FTIR and elemental analysis confirm the formation of cerium zinc molybdate nanoparticles. The conductivity results indicate that conventional synthesis takes longer time, while in sonochemical technique (US), reaction completes within short period of time. Improved solute transfer rate, rapid nucleation, and formation of large number of nuclei are attributed to presence of cavitation. Saturation of the Ce(3+) ions reaches earlier in case of sonochemical technique which restricts the growth of particles hence smaller size is obtained. The crystallite size of cerium zinc molybdate was found to be 27nm from XRD analysis.

Analysis of semibatch emulsion polymerization: role of ultrasound and initiator.

In this work semibatch miniemulsion was carried out wherein the effect of free radicals produced by ultrasound and an external addition of initiator was examined. Influence of different variables on polymerization rate and polymer particle size has also been investigated. Over a range of 0-4% (by wt) initiator, the polymerization rate was found to increase over a range of 0.56-1.33 g L(-1) min(-1). Similarly monomer concentration range (7.2-15 wt.%) changed the polymerization rate from 1.33 to 2.61 g L(-1) min(-1). Under optimum parametric conditions polymer particle size 50 nm were obtained with a narrow size distribution. Syndiotactic phase of PMMA was observed by controlling the formulation recipe. Although, number of reports could be found in the literature [9,13,17,18,20,22] related to batch emulsion polymerization, this experimental data could be useful for the production of large scale monodispersed PMMA latex as all of the scale-up and design parameters have been qualitatively addressed.

Tuning PID controllers for higher-order oscillatory systems with improved performance.

In this paper, model based design of PID controllers is proposed for higher-order oscillatory systems. The proposed method has no limitations regarding systems order, time delays and oscillatory behavior. The reduced model is achieved based on third-order modeling and selection of coefficients through the use of frequency responses. The tuning of the PID parameters are obtained from a reduced third-order model; the procedure seems to be simple and effective, and improved performance of the overall system can be achieved. Three simulation examples and one real-time experiment are included to demonstrate the effectiveness and applicability of the proposed method to systems with oscillatory behavior.

Ultrasound assisted synthesis of polyacrylic acid-nanoclay nanocomposite and its application in sonosorption studies of malachite green dye.

Synthesis of nanoclay nanocomposite has been undertaken by using polyacryalic acid (PAA) in aqueous medium and ultrasound environment and its application in dye removal has been investigated. The synthesized product was characterized by using FTIR and XRD techniques. The sonosorption capacity of the product namely PAA-nanoclay composite was determined by choosing malachite green (MG) dye as a model pollutant. The effects of various parameters such as nanocomposite loading, pH, various process conditions etc. have been studied. On comparing the results obtained with that of nanoclay as an adsorbent, it was found for an initial concentration of 500mg/l, the PAA-nanoclay nanocomposite exhibited higher percentage of pollutant removal (68%) and for nanoclay it was 54%. The adsorption data has been correlated using Langmuir and Freundlich models. The fit of the Freundlich isotherm model was found to be good in the entire range of concentration for the experimental sorption data obtained on the nanoclay nanocomposite. A plausible reaction mechanism for use of PAA-nanoclay nanocomposite as an adsorbent is also proposed.

Some aromatic nitrate esters: synthesis, structural aspects, thermal and explosive properties.

1-(2-Nitroxyethylnitramino)-2,4,6-trinitrobenzene (I-A), 1, 3-bis(2-nitroxyethylnitramino)-2,4,6-trinitrobenzene (II-A) and 1,3, 5-tris(2-nitroxyethylnitramino)-2,4,6-trinitrobenzene (III-A) have been prepared by condensing picryl chloride, styphnyl chloride and 1, 3,5-trichloro-2,4,6-trinitrobenzene with ethanol amine, respectively, followed by nitration. These compounds have been characterized by infrared spectrum (IR), the elemental analysis and 1H NMR. Further, these compounds have been studied for their thermal and explosive properties. The activation energy of thermal decomposition of these compounds has also been determined using the Ozawa and the Kissinger methods. The data on explosive properties indicate that the impact, friction and velocity of detonation (VOD) increase with an increase in the number of nitrate ester groups.