Controlled synthesis of ZnO nanoparticles from a Zn(II) coordination polymer: Structural characterization,optical properties and photocatalytic activity

A zinc coordination polymer derived from pyridine-2,6-dicarboxylate (PDC), {[Zn₂(PDC)₂]}_n, was successfully prepared via conventional, sonication and microwave-irradiation methods. The composition and characteristics of the obtained coordination polymers (CPs) were investigated by elemental analysis, TGA/DTA, X-ray diffraction and spectroscopic techniques. The so obtained CPs were heat-treated in the air at 600 °C for 2 h to produce ZnO of nanosized particles (NPs). It is of interest to note that the synthesis approach of the precursor greatly affects both the nanoparticle size and the structure of the resulting ZnO NPs. Moreover, the smallest particle size was associated with the sample derived from the ultrasonically prepared precursor. TEM analysis revealed that all samples have sphere-like morphologies. Structural analysis of the prepared ZnO samples was conducted and compared using Rietveld analysis of their PXRD patterns. Optical band gap calculations based on analysis of the UV–vis spectra of ZnO samples using Tauc's power law were achieved. The highest band gap of 3.63 eV was observed for ZnO sample obtained from the ultrasonically prepared precursor. Furthermore, the photocatalytic activity of ZnO NPs for the removal of Eosin Y color was monitored. The highest removal efficiency was recorded for ZnO originated from the ultrasonically synthesized precursor. Enhancement of removal efficiency that reached 98% was attained in only a period of 8 min. Its recycling test showed that it can be reused without structural changes over four cycling experiments.     

超声辐射下某些含官能团化合物与二氯卡宾的反应

超声辐射在有机反应中的应用日趋广泛。我们曾报道了超声辐射与相转移催化相结合产生二氯卡宾和二溴卡宾的方法及其与烯烃加成反应的结果。该法比单纯使用相转移催化剂或超声辐射更为可取。本文进一步将它用于二氯卡宾与某些含官能团化合物的反应,考察超声辐射的影响。反应是在固-液两相条件下进行的,即以粉末状氢氧化钠为碱,氯仿过量兼作溶剂。结果表明,超声辐射对各类化合物反应的影响有相当明显的差异。     

Preparation and fabrication of porous-Fe2O3/carbon black nanocomposite: a portable electrochemical sensor for psychotropic drug detection in environmental samples

Herein, we reported the fabrication of porous iron oxide/carbon black (P–Fe₂O₃/CB) composite through a two-step engineering method. At first, Prussian blue microcubes were used as a precursor and further calcined to form P–Fe₂O₃ microcubes. The intercalation of CB nanoparticles with P–Fe₂O₃ nanocubes was processed through the ultrasonication method. The obtained P–Fe₂O₃/CB were successfully scrutinized through various physiochemical characterization methods. The proposed P–Fe₂O₃/CB-modified glassy carbon electrode sensor was successfully implemented in the electrochemical sensing of chlorpromazine hydrochloride due to its very low charge transfer resistance (R_ct) compared to the other electrode modifiers. The sensitive detection of CPMH through differential pulse voltammetry exemplifies an excellent electroanalytical performance such as a wide linear range of 0.5–1472 μM, a lower detection limit (0.001 μM), and an appraisable sensitivity of 1.99 μA/μM cm^?2 due to its availability of a high number of active sites and its large surface area, respectively. It also expresses excellent selectivity, repeatability, reproducibility, and stability results. Moreover, the practical feasibility of the as-fabricated P–Fe₂O₃/CB/glassy carbon electrode sensor shows exquisite recovery (98.1–100.8%) results with an appraisable current response in various biological, pharmaceutical, and environmental samples.     

Process intensification for synthesis of triglycerides of capric acid using green approaches

The present research focuses on intensified synthesis of tricaprin by esterification reaction between capric acid and glycerol catalysed by dry amberlyst-15 using ultrasonication approach. Effect of several reaction conditions like molar ratio, reaction temperature, and amberlyst-15 loading on the rate of conversion has been studied. Effect of ultrasonic conditions like duty cycle and irradiation time on the intensified synthesis is investigated. Recyclability of amberlyst-15 is studied to make process more economical. It is investigated that the optimum reaction conditions which gave maximum conversion of 95% were molar ratio of capric acid: glycerol as 3:5, reaction temperature 90 ​°C, 4% amberlyst −15 loading. It was further investigated that ultrasonic conditions which gave intensified synthesis were 70% duty cycle and irradiation time of 120 ​min. The ultrasonic assisted process was compared with conventional synthesis. Conventional synthesis gave 30% yield in 120 ​min and 82% in 18 ​h. Amberlyst-15 was successfully reused for 13 cycle without any change in the conversion (%) of reaction.     

One-pot multicomponent synthesis of unsymmetrical polyhydroquinoline derivatives with 1,1’-butylenebispyridinium hydrogen sulfate as an efficient,halogen-free and reusable Brönsted ionic liquid catalyst

1,1''-Butylenebispyridinium hydrogen sulfate is an efficient, halogen-free and reusable Brönsted ionic liquid catalyst for the synthesis of ethyl-4-aryl/heteryl-hexahydro-trimehtyl-5- oxoquinoline-3-carboxylates by the one-pot condensation of dimedone, aryl/heteryl aldehydes, ethyl acetoacetate, and ammonium acetate under solvent-free conditions. This method has the advantages of high yield, clean reaction, simple methodology, and short reaction time. The ionic liquid can be recycled five times without significant loss of the catalytic activity.     

Ultrasonic cavitation at liquid/solid interface in a thin Ga–In liquid layer with free surface

Cavitation in thin layer of liquid metal has potential applications in chemical reaction, soldering, extraction, and therapeutic equipment. In this work, the cavitation characteristics and acoustic pressure of a thin liquid Ga–In alloy were studied by high speed photography, numerical simulation, and bubble dynamics calculation. A self-made ultrasonic system with a TC4 sonotrode, was operated at a frequency of 20 kHz and a max output power of 1000 W during the cavitation recording experiment. The pressure field characteristic inside the thin liquid layer and its influence on the intensity, types, dimensions, and life cycles of cavitation bubbles and on the cavitation evolution process against experimental parameters were systematically studied. The results showed that acoustic pressure inside the thin liquid layer presented alternating positive and negative characteristics within 1 acoustic period (T). Cavitation bubbles nucleated and grew during the negative-pressure stage and shrank and collapsed during the positive-pressure stage. A high bubble growth speed of 16.8 m/s was obtained and evidenced by bubble dynamics calculation. The maximum absolute pressure was obtained at the bottom of the thin liquid layer and resulted in the strongest cavitation. Cavitation was divided into violent and weak stages. The violent cavitation stage lasted several hundreds of acoustic periods and had higher bubble intensity than the weak cavitation stage. Cavitation cloud preferentially appeared during the violent cavitation stage and had a life of several acoustic periods. Tiny cavitation bubbles with life cycles shorter than 1 T dominated the cavitation field. High cavitation intensities were observed at high ultrasonication power and when Q235B alloy was used because such conditions lead to high amplitudes on the substrate and further high acoustic pressure inside the liquid.     

Effect of ultrasound and chlorine dioxide on Salmonella Typhimurium and Escherichia coli inactivation in poultry chiller tank water

This study evaluated the application of ultrasound alone or combined with chlorine dioxide (ClO₂) for Salmonella Typhimurium and Escherichia coli inactivation in poultry processing chiller tank water. A Full Factorial Design (FFD) 2² was conducted for each microorganism to evaluate the effect of ultrasound exposure time (x₁: 1 to 9 min; fixed: 37 kHz; 330 W; 25 °C) using a bath, and ClO₂ concentration (x₂: 1 to 17 mg L⁻¹) on microorganism count expressed in log CFU mL⁻¹ in distilled water. Variable x₂ had a negative effect on Salmonella Typhimurium (-5.09) and Escherichia coli (-2.00) count, improving the inactivation; while a x₁ increase present no inactivation improvement, explaining the use of x₁ lower level (1 min) and x₂ higher level (17 mg L⁻¹). The best condition for microorganism inactivation based on FFD was evaluated in chiller tank water (with organic matter) at 25, 16, and 4 °C; x₁ was kept (1 min), however x₂ was adjusted to obtain the same residual free chlorine (2.38 mg L⁻¹) considering the ClO₂ consumption by organic matter, achieving the value of 30 mg L⁻¹. An inactivation of 49% and 31% were observed for Salmonella Typhimurium and Escherichia coli. When ultrasound was replaced by a simple agitation in the presence of ClO₂, there was no inactivation for both microorganisms. Moreover, at poultry carcass pre-chilling (16 °C) and chilling (4 °C) conditions, the synergism of ultrasound combined with ClO₂ was more pronounced, with microorganisms’ reductions up to 100%.     

Research for improvement on the extract efficiency of lignans in traditional Chinese medicines by hybrid ionic liquids: As a case of Suhuang antitussive capsule

Recently, efficient extraction of natural products from traditional Chinese medicines (TCMs) by green solvents is deemed an essential area of green technology and attracts extensive attentions. In this work, a green protocol for simultaneous ultrasonic-extraction of the native compounds with different polarities of TCMs by using a hybrid ionic liquids (HILs)-water system was reported for the first time. As a case study, three superior ILs (1-ethyl-3-methylimidazolium tetrafluoroborate ([EMIM][BF4]), 1-ethyl-3-methylimidazolium acetate ([EMIM][OAc]), and 1-allyl-3-methylimidazolium chloride ([AMIM]Cl)) were chosen as the compositions of the HILs system, and the TCMs Suhuang antitussive capsule (SH) containing different-polarity lignans was selected. Primarily, an ultra-performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry (UPLC-QqQ-MS/MS) method in the multiple reaction monitoring (MRM) mode was established for qualitative and quantitative analysis of 18 lignans. After majorization by uniform design experiment, the HILs prepared with [AMIM]Cl, [EMIM][BF4], and [EMIM][OAc] at a volume ratio of 1:5:5 could simultaneously extract multi-polarity lignans compared to single IL. Subsequently, the conditions of ultrasonic extraction employing with HILs and traditional organic solvent were optimized by the response surface methodology, respectively. The results indicated that the extract efficiency of the HILs system for target compounds was significantly improved compared with the traditional organic solvent-extraction, i.e. the content of total lignans in ethanol system was up to 47 mg/g, while that in the HILs system was up to 69 mg/g, with an increasing of 47%. Additionally, ¹H-NMR and ¹³C-NMR spectra were used to characterize the hydrogen-bond interactions in the HILs-lignan mixtures. Extraction with the HILs in TCMs is a new application schema of ILs, which not only avoids the use of volatile toxic organic solvents, but also shows the potential to be comprehensively applied for the extraction of bioactive compounds from TCMs.     

Rheological insights on the evolution of sonicated cellulose nanocrystal dispersions

Cellulose nanocrystals (CNCs) are promising biomaterials, but their tendency to agglomerate when dried limits their use in several applications. Ultrasonication is commonly used to disperse CNCs in water, bringing enough energy to the suspension to break agglomerates. While the optimized parameters for sonication are now well defined for small volumes of low concentration CNC suspensions, a deeper understanding of the influence of the dispersing process is needed to work with larger volumes, at higher concentrations. Herein, rheology is used to define the distribution and dispersion states upon ultrasonication of a 3.2 wt% CNC suspension. After considering the importance of the measurement sampling volume, the behavior of a more concentrated suspension (6.4 wt%) is examined and compared with a never-dried suspension of the same concentration to validate the dispersion state.