Ultrasound Irradiation Method Research Articles

Ultrasound assisted synthesis of hybrid quinoline anchored with 4-R-benzenesulfonamide moiety with potential antimicrobial activity

We present in this paper a direct and efficient study regarding synthesis and spectral characterization of three series of hybrid quinoline anchored with 4-R-benzenesulfonamide moiety, with potential antimicrobial activity, by using ultrasound (US) irradiation and conventional methods (CV). The synthesis pathway is efficient and direct, in two steps: an initial N-acylation of 8-aminoquinoline followed by metal complexation with variously M2+ metals (Cd2+, Co2+, Cu2+, Ni2+, Pd2+, Zn2+). For both type of reactions, N-acylation and complexation, under US irradiations the synthesis have some undeniable advantages: the most relevant being the higher yields, a dramatically decrease for reaction time (with about 150 (one hundred fifty) folds for complexation) comparative with conventional methods (CV) (therefore the spent energy decrease in the same way), a decrease of the amount of used solvents. Taking into account the above considerations these reactions setup could be appreciated as eco-friendly. The structures of the obtained hybrid quinoline – sulfonamide complexes (HQBSM) were determined by elemental analysis and by using spectral investigations: FT-IR, NMR experiments, and X-ray diffraction (in three cases). The FT-IR and NMR spectra of complexes show a similar spectroscopic pattern for all complexes and fully confirm the proposed structures. The X-ray spectra analyses prove without doubts the structure of metal complexes, indicating that their structure depends essentially by two factors: the nature of metal and the nature of sulfonamide-quinoline moieties. Complexes containing 4-methoxy-benzoyl moiety and Zn2+ (e.g. 6a) are tetra-coordinated while in the Ni2+ complex (e.g. 6e) the metallic ion forms a distorted square-based bi-pyramid. In the complexes containing 4-nitro-benzoyl moiety and Cd2+ (e.g. 5d) the metallic ion forms a triangular bipyramid. The antibacterial and antifungal assay reveal that only hybrid HQBSM complex (4e) (with 4-chlorophenyl moiety and Ni2+ in molecule) have a significant antibacterial activity.

Rapid synthesis of hierarchical cerium-based metal organic frameworks for carbon dioxide adsorption and selectivity

The creation of innovative porous materials for CO2 capture and separation is proving extremely relevant for environmental sustainability and global warming mitigation. In this study, modified Ce-UiO-66 MOFs were synthesized in 10 min using simultaneous microwave and ultrasound irradiation method. The porosity of the MOF was altered using the soft-templating approach. This strategy resulted in the construction of a hierarchically micro-mesoporous structure with an average mesopore size of 11.10 nm. The as-obtained MOFs, abbreviated as CUT, were characterized with SEM, XRD, FTIR, TGA, BET, and evaluated as CO2 adsorbents. The results displayed preserved crystal structure, higher thermal stability up to 570 °C. The heightened diffusion of CO2 molecules to the micropores promoted by mesopore channels, endued CUT with an over-all CO2 adsorption uptake of 2.53 mmol/g at 273 K at 1 bar outperforming equivalent Ce-UiO-66 MOFs. Notably, the CUT adsorbent showed improved CO2/N2 IAST selectivity (34.2 vs 24.6) and CO2 isosteric heat of adsorption (Qst = 30.15 vs 25 kJ/mol) in contrast to pristine UiO-66 (Zr).

Water mediated pot, atom, and step economic (PASE) synthesis of pyrimido[4,5-d]pyrimidines using ultrasound and microwave irradiation approaches

The functioning, Pot, Atom, and Step Economic (PASE) green chemistry proposition has been approached for the synthesis of pyrimido[4,5-d]pyrimidines by the multicomponent reaction (MCR) of barbituric acid, guanidine, and aldehyde derivatives using water solvent and iodine catalyst through ultrasound and microwave irradiation methods. Reaction optimization was performed by varying solvents, reaction time, the concentration of catalyst, and reaction methods. Microwave irradiation approach using water solvent and iodine catalyst (8 mol%) with 5 min led to offer the highest yield. EWG substituted compound 4 g (4-NO2, guanidine) [87% (U.S.), 93% (M.W.)] was found to be the highest yielded compound in this study. The greenness of the reaction was estimated by calculating some green chemistry metrics. The metrics approved the proposed protocol as an ideal, green, and sustainable approach.

Structural Analysis of Calcium Oxide Derived from Waste Egg’s Shells and their Application for Knoevenagel Condensation Reactions

The present study demonstrates the simple and easy synthesis of calcium oxide (CaO) from waste egg’s shells. Fine egg’s shells powder were calcinated at 500, 700 and 800 ºC. The structural and morphological evaluation of calcium oxide derived from waste egg’s shell were examined by using XRD, FT-IR, SEM, EDS and TEM techniques. The sintered calcium oxide was used as heterogeneous catalyst for the synthesis of 5-arylidene malononitrile and 5-arylidene barbituric acid derivatives by the condensation of various aromatic aldehyde and active methylene compounds via Knoevenagel condensations reaction under ultrasound irradiation method. The reaction completed within a very short reaction time with high yields of product. The present method describes easy synthesis of calcium oxide catalyst from the waste egg’s shells, short reaction times, simple product isolation, excellent yield and reusability of the catalyst.

Green synthesis and antimicrobial activity of 1,3-diaryl pyrazole based chalcone derivatives

We report a facile green synthetic protocol for the synthesis of 1,3-diaryl pyrazole based chalcone derivatives by the condensation of 3-Aryl-1-phenyl-1Hpyrazole- 4-carbaldehydes with arylmethylketones in the presence of base in both microwave and ultrasound irradiation method. The synthesized compounds were evaluated for in vitro antimicrobial activity against four bacterial organisms and two fungal organisms showing moderate to good activity.

Insights into the luminescent properties of poly(phenylene sulfide)-grafted metal-organic framework (Tb–MOF–PPS) copolymers

In this study, a novel poly(phenylene sulfide)-grafted metal-organic framework (Tb–MOF–PPS) was fabricated. Initially, 2,5-dichloroterephthalic acid and TbCl3·6H2O were used as raw materials to synthesize the dihalogenated MOF (Tb–MOF) through ultrasound irradiation and hydrothermal methods. Subsequently, Tb–MOF was added at different mole proportions (2.5, 5, 7.5, and 10%) for the copolymerization of PPS, and a serial of Tb–MOF–PPS composites were successfully obtained. Fourier transform infrared spectroscopy, X-ray diffraction, and X-ray photoelectron spectroscopy proved that the Tb–MOF was covalently connected to PPS. The introduction of the Tb–MOF had no evident influence on the thermal properties of the composites. Additionally, the fluorescence characteristics revealed that the fluorescence excitation and emission spectra of the composites had a large redshift compared with that of PPS and possessed visible-light photoluminescence properties. These results indicate that the composites obtained can be used as optical sensors.

Using Microwave and ultrasound to prepare of substituted Bis-acyl hydrazone Derivatives

Abstract In this paper, some new bis-aryl hydrazone derivatives (4a-f) were prepared through the reaction of carboxylic acid hydrazides with 1,4-diacetylbenzene using classical methods, microwave and ultrasound irradiation methods. These compounds are obtained through a series of reactions where some carboxylic acids react with ethanol first in the presence of concentrated sulfuric acid to give the corresponding esters (2a-f), which when treatment with aqueous hydrazine give carboxylic acid hydrazides (3a-f).thus, The results proved that the use of microwave and ultrasound techniques is much better than the classical methods, as it gave a higher yield, shorter reaction time, and the absence of the use of solvents. All newly synthesized compounds were confirmed by IR, (1H & 13C) NMR spectral analysis and the corresponding reactions were monitored by TLC using the reported eluent

Effect of low intensity pulsed ultrasound on osteoclast differentiation

ABSTRACT Purpose For many years, people have attempted to identify ways of efficiently moving teeth in orthodontic therapy to reduce harmful effects. In this study, we investigate whether the non-surgical method of low-intensity pulsed ultrasound (LIPUS) irradiation affects osteoclast differentiation in vitro. Materials and Methods RAW264 cells were stimulated with RANKL and U0126, and LIPUS irradiation was performed using different ultrasonic outputs, irradiation times, and number of irradiations. Assessments used TRAP staining, TRAP quantitative assays, and western blot analysis. Results LIPUS irradiation significantly increased osteoclast differentiation rates of RAW264 cells. The rates were significantly higher in the three-time irradiation group compared with the single irradiation group. However, significant differences were not observed between the ultrasonic output. TRAP quantitative assay results showed significantly increased osteoclast differentiation rates with increased irradiation time, however, only in the single irradiation group. Conclusion These results suggest that an increased number of LIPUS irradiations may improve its effectiveness in orthodontic therapy.

Highly sensitive detection of environmental pollutant cadmium with ultrasonic irradiated Pt-supported ZSM-5 modified electrode

Abstract A glassy carbon electrode (GCE) was modified with platinum (Pt)-supported ZSM-5 (GCE/ZSM-5/Pt) prepared by an ultrasonic-assisted hydrothermal method and applied to the electrochemical detection of cadmium (Cd2+) ions. Ultrasonic preparation method is an emerging green technique for the preparation of active catalyst materials with an enhanced optical, electrical and morphological properties. The ZSM-5/Pt (2.4–50%) catalyst was prepared by the ultrasound irradiation method. During this preparation, the ultrasonic irradiation time, ultrasonic sources, power density, stirring, and reactor temperature were considered. The intrinsic and extrinsic properties of ZSM-5/Pt (2.4–50%), such as the surface area, pore volume, particle size, pore diameter and crystallinity could be controlled by the ultrasonic-assisted method. The prepared electrode material was investigated with physical and chemical characterization techniques. The GCE/ZSM-5/Pt (5.4%) modified electrode expressed higher electrocatalytic activity than other modified electrodes for the determination of Cd2+ ions. Analytical factors of the electrochemical sensor, such as deposition time, pH, and deposition potential, were estimated by differential pulse voltammetry (DPV). The GCE/ZSM-5/Pt (5.4%) modified electrode had a low limit of detection (0.012 μM), wide linear range (0.1–7.2 μM), high sensitivity (17.639 μAμMcm−2), high stability, and high reproducibility. Hence, the GCE/ZSM-5/Pt (5.4%) electrode sensor can be applied for sensing hazardous Cd2+ metal ions in environmental water samples with appreciable recovery.

Ultrasound‐assisted synthesis of substituted triazines and their corrosion inhibition behavior on N80 steel/acid interface

AbstractThe three substituted triazines were synthesized by ultrasound irradiation method and characterized by FTIR, 13C NMR, and 1H NMR. The corrosion inhibition behavior of the synthesized inhibitors on N80 steel in 15% HCl was studied using electrochemical analyses and weight loss methods. All three inhibitors exhibited excellent corrosion inhibition performance, and the best inhibition effect was shown by TZ‐3 (93.2% at 800 mg/L). EIS measurements suggest that the corrosion inhibition process is a charge transfer controlled. The PDP results indicated that all the triazines are mixed‐type inhibitors. Langmuir adsorption model is the best fit among the other tested isotherms. These molecules can act as promising acidizing corrosion inhibitors for the oil gas industry. FTIR, AFM, and UV‐vis studies corroborate the adsorption of inhibitor molecules over the metal surface.

SnO2 Quantum Dots Interspersed d-Ti3C2Tx MXene Heterostructure with Enhanced Performance for Lithium Ion Battery

Ti3C2Tx MXene is an important concern for lithium ion batteries (LIB) because of its two-dimensional (2D) open structure, excellent electrical conductivity, and low Li+ diffusion barrier. However, MXene anodes have a lower capacity, which limits their further application in LIBs. This study presents a SnO2 QDs@delaminated Ti3C2Tx (d-Ti3C2Tx) heterostructure composite that is produced via in situ growth of SnO2 QDs on the layer of d-Ti3C2Tx nanosheets and uses a facile ultrasound irradiation method. Results illustrate that SnO2 QDs are uniformly anchored on the surface of d-Ti3C2Tx layer. The d-Ti3C2Tx nanosheets inhibits the agglomeration of SnO2 QD nanoparticles and volume expansion during the charging-discharging process. The hierarchical structure can enlarge the interface area of electrode and electrolyte, which accelerating Li-ion and electron diffusion and transition processes. Electrochemical results reveal that compared to pure d-Ti3C2Tx and SnO2 QDs, SnO2 QDs@d-Ti3C2Tx nanocomposites greatly improve the reversible capacity. Remarkably, the SnO2@d-Ti3C2Tx composite maintains 390 mAh·g−1 with a capacity recovery after 100 cycles at current density of 1000 mA·g−1. The synergistic effect of SnO2 QDs on MXene prevents the re-stacking of d-Ti3C2Tx layers and increases the Li+ storage; thus, this system exhibits excellent electrochemical properties for LIBs.

Synthesis and bioassay of a new class of disubstituted 1,3,4-oxadiazoles, 1,3,4-thiadiazoles and 1,2,4-triazoles

A new class of aroylethenesulfonylmethyl styryl oxadiazoles/thiadiazoles/triazoles and arylsulfonylethenesulfonylmethyl styryl oxadiazoles/thiadiazoles/triazoles were synthesized from the synthetic intermediates E-aroylethenesulfonylacetic acid methyl ester, E-arylsulfonylethenesulfonylacetic acid methyl ester and substituted cinnamic acids adopting conventional and ultrasonication methodologies. All the synthesized compounds were obtained in higher yields and in shorter reaction times in ultrasound irradiation method when compared with conventional method. The structures of all the compounds were characterized by IR, 1H NMR, 13C NMR and mass spectra. All the title compounds were tested for antimicrobial activity. The arylsulfonylethenesulfonylmethyl styryl azoles displayed higher antimicrobial activity than the aroylethenesulfonylmethyl styryl azoles. The compounds having triazole moiety showed greater activity than those with oxadiazole and thiadiazole. Amongst all the tested compounds unsubstituted and chloro substituted arylsulfonylethenesulfonyl methyl styryl triazoles are identified as potential antimicrobial agents particularly against B. subtilis and P.chrysogenum.

Combination of precipitation and ultrasound irradiation methods for preparation of lanthanum-modified Y zeolite nano-catalysts used in catalytic cracking of bulky hydrocarbons

Abstract In the present study, lanthanum-containing HY nano-catalysts were prepared using three different techniques including wet impregnation, precipitation, and new precipitation-ultrasonic methods for the sake of catalysts performance promotion through improvement of rare earth dispersion on zeolite. The synthesized nano-catalysts were characterized by means of XRD, N2 adsorption-desorption, TEM, NH3-TPD, FE-SEM and EDX dot-Mapping techniques. Furthermore, amount and type of deposited coke over the spent nano-catalysts were investigated using TGA and FT-IR analyses, respectively. N2 adsorption-desorption analysis showed that the textural properties of zeolite were acceptably preserved in the prepared nano-catalyst with precipitation-ultrasonic method. TEM and EDX dot-Mapping analyses indicated that using ultrasonic irradiation led to synthesis well-dispersed and smaller size lanthanum species over the Y zeolite. Obtained results from the catalytic performance of nano-catalysts revealed that compared with impregnation and precipitation methods, using precipitation-ultrasonic technique not only led to achievement of significantly higher gasoline yield (increase 41% in comparison to parent catalyst), but also efficient decrease in density, viscosity and molecular weight of liquid product were obtained. In addition, application of precipitation-ultrasonic method moderated the acidity strength of zeolite. It led to increased nano-catalyst life time and less coke formation.

Synthesis, characterization, and bioassay of a new class of pyrazolyl/isoxazolyl oxadiazoles

This study aimed at describing a simple and facile synthesis of pyrazolyl/isoxazolyl 1,3,4-oxadiazole derivatives from the synthetic intermediates pyrazolyl/isoxazolyl carboxylates adopting conventional and ultrasound irradiation methods. In fact ultrasound-promoted synthesis led to the formation of title compounds in higher yields and in shorter reaction times when compared with conventional methods. All the compounds were characterized by IR, 1H NMR, 13C NMR, and mass spectra. The synthesized compounds were evaluated for their antioxidant and anti-inflammatory activities. The bioassay results indicated that some title compounds were found to be more potent than standard drugs. Amongst all the tested compounds furanyl/pyridinyl linked pyrazolyl/isoxazolyl methoxyphenylsulfonylmethyloxadiazoles were identified as potential antioxidant and anti-inflammatory agents.

Synthesis and characterization of nano-sized metal organic framework-5 (MOF-5) by using consecutive combination of ultrasound and microwave irradiation methods

Nano-sized metal organic framework-5 (MOF-5) was prepared in the presence of triethylamine (TEA) via consecutive combination of ultrasound (US) and microwave irradiation (MW) methods by exploiting the benefit of obtaining MOF-5 in very short reaction times (∼2 min) and high yields (∼95%). The surface area of MOF-5 was found to be 1203 m2/g. The highly crystalline structure of nano-sized MOF-5 was confirmed by XRD. Vibrational modes and thermal decomposition behavior of nano-sized MOF-5 were verified from ATR FT-IR and TGA results, respectively. Based on SEM and AFM results, MOF-5 nanoparticles are spherical in shape, and their sizes vary in the range of 20–80 nm. The high purity of nanosized MOF-5 was confirmed by XRD and EDS results. A very regular and homogenous distribution of MOF-5 nanoparticles with a size range of 20–30 nm within poly(ethylene oxide) (PEO) electrolyte was clearly observed from SEM results. The reason behind size reduction and homogenous distribution of nano-sized MOF-5 was stated as the elimination of any possible aggregation of MOF-5 nanoparticles due to favorable physical interactions between PEO and surface functional groups of MOF-5 during the solution casting process.

Hierarchically three-dimensional (3D) nanotubular sea urchin-shaped iron oxide and its application in heavy metal removal and solar-induced photocatalytic degradation

In this study, hierarchically three-dimensional (3D) nanotubular sea urchin-shaped iron oxide nanostructures (3D-Fe2O3) were synthesized by a facile and rapid ultrasound irradiation method. Additives, templates, inert gas atmosphere, pH regulation, and other complicated procedures were not required. Dense 3D-Fe2O3 with a relatively large Brunauer–Emmett–Teller (BET) surface area of 129.4 m2/g was synthesized within 23 min, and the BET surface area was further improved to 282.7 m2/g by a post heat-treatment process. In addition, this post processing led to phase changes from maghemite (γ phase) to hematite (α phase) Fe2O3. Subsequent characterization suggested that the growth mechanism of the 3D-Fe2O3 follows self-assembly and oriented attachment. The prepared 3D-Fe2O3 was applied to wastewater purification. Ultrasound-irradiated 3D-Fe2O3 can eliminate a As(V) and Cr(VI) from water with 25 times faster removal rate by using a one third smaller amount than commercial α-Fe2O3. This was attributed to the inter-particle pores and relatively positively charged surface of the nanostructure. In addition, post heat treatment on ultrasound-irradiated 3D-Fe2O3 significantly influenced the photocatalytic degradation of methylene blue and phenol, with a 25 times higher removal efficiency than that of commercial α-Fe2O3, because of both high BET surface area and good crystallization of the prepared samples.

Synthesis of some new pyrrolyl dipyrazoles and pyrrolyl pyrazolyl isoxazoles and biological evaluation as antioxidants

Some new systems of tris-heterocyclic pyrrolyl dipyrazoles (5) and pyrrolyl pyrazolyl isoxazoles (7) were prepared from the Michael acceptor E-1-(4-aryl-1H-pyrazol-3-yl)-3-(1H-pyrrol-2-yl)prop-2-en-1-one (3) using conventional and ultrasonication methods. All compounds were obtained in higher yield and shorter reaction time when using the ultrasound irradiation method compared with the conventional method. The title compounds were assayed for their antioxidant activity. Amongst all the tested compounds, 5c and 7c exhibited pronounced antioxidant activity compared with the standard drug.

Antimicrobial, anticoagulant, and cytotoxic evaluation of multidrug resistance of new 1,4-dihydropyridine derivatives.

A new series of 1,4-dihydropyridine derivatives (2a–h, 3a–e, and 4a–e) were systematically designed and synthesized via ultrasound irradiation methods with easy work-up and good yields. Compounds structures were confirmed by IR, 1H NMR, 13C NMR, and mass spectra. The synthesized compounds were screened for both antimicrobial and anticoagulant activities. Compound 2e (MIC: 0.25 μg/mL) was highly active against Escherichia coli and compound 2c (MIC: 0.5 μg/mL) was also highly active against Pseudomonas aeruginosa compared with ciprofloxacin. (MIC: 1 μg/mL) The antifungal activity of 2c (MIC: 0.5 μg/mL) against Candida albicans was high relative to that of clotrimazole (MIC: 1 μg/mL). Anticoagulant activity was determined by activated partial thromboplastin time (APTT) and prothrombin time (PT) coagulation assays. Compound 4-(4-hydroxyphenyl)-2,6-dimethyl-N3,N5-bis(5-phenyl-1,3,4-thiadiazol-2-yl)-1,4-dihydropyridine-3,5-dicarboxamide 3d (>1000 s in APTT assays) was highly active in anticoagulant screening compared with the reference of heparin.Cytotoxicity was evaluated using HepG2 (liver), HeLa (cervical), and MCF-7 (breast) cancer cell lines, with high toxicities observed for 2c (GI50 = 0.02 μm) against HeLa cell line and 2e (GI50 = 0.03 μm) equipotant against MCF-7 cell line. Therefore, the compounds 2e, 2c and 3d can serve as lead molecules for the development of new classes of antimicrobial and anticoagulant agent.

BDF Synthesis based on Environment-friendly Ultrasound Irradiation Method

BDF Synthesis based on Environment-friendly Ultrasound Irradiation Method

Synthesis and antimicrobial activity of pyrimidinyl 1,3,4-oxadiazoles, 1,3,4-thiadiazoles and 1,2,4-triazoles

A new class of methylthio linked pyrimidinyl 1,3,4-oxadiazoles, 1,3,4-thiadiazoles and 1,2,4-triazoles were prepared under conventional and ultrasound irradiation methods. All the compounds were obtained in higher yields and in shorter reaction times in ultrasound irradiation method when compared with the conventional method. The title compounds were tested for antimicrobial activity. The compounds 12c and 12f exhibited promising antibacterial activity against P. aeruginosa whereas the compounds 13c and 13f showed pronounced antifungal activity against A. niger.