3-芳亚甲基吲哚-2-酮类化合物的合成及其抑菌活性研究

在超声辐射和哌啶催化反应条件下,1,3-二氢吲哚-2-酮(1)与芳香醛2a~2m发生Knoevenagel缩合反应,合成了一系列3-芳亚甲基吲哚-2-酮衍生物3a~3m。该方法具有产率高、反应时间短、后处理简单和环境友好等优点,产物通过~1H NMR、~(13)C NMR和HRMS手段进行结构表征,并通过核磁2D NOESY确定了所有化合物几何构型。初步抑菌活性测试结果表明,化合物3d对革兰氏阳性菌具有较好的抑制作用,最小抑菌浓度(MIC)为15.6μg/m L,化合物3f、3g、3h和3k对油菜菌核病菌表现出良好的抑制活性,MIC为62.5μg/m L,与阳性对照多菌灵相当。此外,对此类化合物的构效关系进行了讨论。     

微波辅助萃取与超声波萃取丹参中丹酚酸B的比较研究

本文对微波辅助萃取和超声波萃取丹参中丹酚酸B进行了比较研究,并用高效液相色谱法(HPLC)测定了丹参中丹酚酸B.考察了微波辅助萃取和超声波萃取参数的影响,在各自最佳萃取条件下进行了丹参中的丹酚酸B提取率的比对,结果表明:微波辅助萃取6 min的提取率高于超声波萃取30 min的提取率.微波辅助萃取法与超声波萃取法相比具有省时、高效和溶剂用量少的特点.利用指纹图谱比较了两种萃取方式提取的化学成分的差异,结果显示两种萃取方法提取的主要成分组成基本相同,其共有成分比例相近.     

Ultrasonic and Raman Scattering Spectroscopy of Zinc Thiocyanate Complexes in Water at 25<Superscript>∘</Superscript>C: Kinetics of Complex Formation Determined by Multivariate Analysis

Advances have been made recently in broadening the accessible ultrasonic absorption frequency range and improving the detectability of minor species present in solution using Raman spectroscopy. Development of chemometric techniques in these areas needs to keep pace with the improvement of these experimental methods. Refinements in the analysis of ultrasonic and Raman data based on multivariable least squares and factor analysis, respectively, are examined to investigate the kinetics of zinc thiocyanate complex formation in water. Analysis of ultrasonic absorption relaxation spectra verified that the observed process in aqueous Zn(SCN)₂ involves substitution of water from the first coordination shell of Zn²⁺. Use of a multivariable least-squares error surface is described that enhances the reliability of assigned frequencies of ultrasonic absorption maxima. Factor analysis of Raman scattering data provided direct evidence that at least four complex species, such as Zn(SCN)⁺ and Zn(SCN)₂, are simultaneously present in the aqueous zinc thiocyanate solutions.     

超声法制备碳量子点发光性能的影响因素分析

超声法制备碳量子点过程简单,成本低廉,不易产生二次污染,应用前景广泛。为优化超声法制备碳量子点的各工艺参数,制备了关键工艺参数不同的碳量子点样品,测试其发射与激发光谱,分析了量子点浓度,溶剂种类,辅助剂种类、浓度,超声功率、时间等参数对碳量子点发光性能影响。结果表明超声法制备的碳量子点具有激发光波长依赖性,发射峰位置随激发波长的变化而发生明显改变;碳量子点浓度增加,发光强度由于非辐射能量传递和团聚作用,先增大后减小;由于溶剂效应,碳量子点在乙醇中比在水中发光强度更强,波长更短,且浓度越大时波峰移动越明显;相比盐酸,以NaOH为辅助剂制备的碳量子点表面钝化程度高,发光强度强;增加辅助剂NaOH浓度可提高量子点表面钝化程度,增大发光强度;同等时间下增加超声功率或同等功率下适量增加超声时间,可制备更多的碳量子点样品,但超声时间过长,碳量子点容易发生团聚猝灭现象。以上影响因素分析为超声法制备碳量子点的工艺参数优化提供了理论基础,有利于碳量子点大规模低成本的生产应用。     

Effect of ultrasonic irradiation on structure and electrochemical properties of LiMn2O4 thin films cathode material for Li-ion micro-batteries

Two kinds of spinel LiMn₂O₄ thin film for lithium ion micro-batteries were successfully prepared on polycrystal Pt substrates by spin coating methods, which were carried out under ultrasonic irradiation (USG) and magnetic stirring (MSG), respectively. The microstructures and electrochemical performance of LiMn₂O₄ thin films were characterized by thermogravimetry analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and galvanostatic charge-discharge measurements. It was found that the crystalline structure of USG samples grew better than that of the MSG samples. At the same time, higher discharge capacity and better cycle stability were obtained for the LiMn₂O₄ thin films of USG at the current density of 50 μAh/cm² between 3.0 and 4.3 V. The 1st discharge capacity was 57.8 μAh/cm²-μm for USG thin films and 51.7 μAh/cm²-μm for MSG thin films. After 50 cycles, 91.4% and 69% of discharge capacity could be retained respectively, indicating that ultrasonic irradiation condition during spin coating was more suitable for preparing spinel LiMn₂O₄ thin films with better electrode performance for lithium ion micro-batteries.     

Numerical study on the desorption processes of oil droplets inside oil-contaminated sand under cavitation micro-jets

The removal of the adsorbed oil droplet is critical to deoiling treatment of oil-bearing solid waste. Ultrasonic cavitation is regarded as an extremely useful method to assist the oil droplets desorption in the deoiling treatment. In this paper, the effects of cavitation micro-jets on the oil droplets desorption were studied. The adsorbed states of oil droplets in the oil-contaminated sand were investigated using a microscope. Three representative absorbed states of the oil droplets can be summarized as: (1) the individual oil droplet adsorbed on the particle surface (2) the clustered oil droplets adsorbed on the particle surface; (3) the oil droplet adsorbed in a gap between particles. The micro-jet generation during the bubble collapse near a rigid wall under different acoustic pressure amplitudes at an ultrasonic frequency of 20 kHz was investigated numerically. The desorption processes of the oil droplets at the three representative absorbed states under micro-jets were also simulated subsequently. The results showed that the acoustic pressure has a great influence on the velocity of micro-jet, and the initial diameter of cavitation bubbles is significant for the cross-sectional area of micro-jets. The wall jet caused by a micro-jet impacting on the solid wall is the most important factor for the removal of the absorbed oil droplets. The oil droplet is broken by the jet impinging, and then it breaks away from the solid wall due to the shear force generated by the wall jet. In addition to a higher sound pressure, the cavitation bubble at a larger initial diameter is more important for the desorption of the clustered oil droplets. Conversely, the micro-jet generated by the cavitation bubble at a smaller initial diameter (0.1 mm) is more appropriate for the desorption of the oil droplet in a narrow or sharp-angled gap.     

Study on rectangular ultrasonic radiator of flexural resonant vibration in high modes

Based on the theory of coupling vibration and flexural vibration of thin rod of rectangular cross section, the fiexural vibration of rectangular thin plate was studied. The frequency equation was derived under the condition of freeboundaries. The normal modes and the relation between the normal modes and the resonant frequency were obtained. Experiments showed that the calculated resonant frequencies agree well with the measured results, and the rectangular thin plate in flexural vibration has abundant resonant frequencies. The radiator of flexural vibration used in ultrasonic cleaning and other techniques has the advantages of large acoustic radiating area, uniform acoustic field and easy adjustment of resonant frequencies, proving that it is a promising ultrasonic source.     

Facile synthesis of calcium silicate hydrate using sodium dodecyl sulfate as a surfactant assisted by ultrasonic irradiation

Calcium silicate hydrate (CSH) consisting of nanosheets has been successfully synthesized assisted by a tip ultrasonic irradiation (UI) method using calcium nitrate (Ca(NO₃)·4H₂O), sodium silicate (Na₂SiO₃·9H₂O) and sodium dodecyl sulfate (SDS) in water. Systematic studies found that reaction time of ultrasonic irradiation and concentrations of surfactant (SDS) in the system were important factors to control the crystallite size and morphologies. The products were characterized by X-ray power diffraction (XRD), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectrometry (FTIR). The size–strain plot (SSP) method was used to study the individual contributions of crystallite sizes and lattice strain on the peak broadening of the CSH. These characterization techniques revealed the successful formation of a crystalline phase with an average crystallite size of about 13 nm and nanosheet morphology at a reaction time of 10 min UI with 0.2 g SDS in solvent which were found to be optimum time and concentrations of SDS for the synthesis of CSH powders.     

Spectrophotometric determination of carbon tetrachloride via ultrasonic oxidation of iodide accelerated by dissolved carbon tetrachloride

Ultrasonic oxidation of iodide was investigated in the presence of carbon tetrachloride (CCl₄). The ultrasonic oxidation of potassium iodide led to formation of iodine and then I₃⁻ in the presence of excess iodide, and the generated I₃⁻ shows strong UV absorption with a molar absorptivity of 2.31 × 10⁴ L mol⁻¹ cm⁻¹ at the maximum absorption wavelength of 351 nm. The ultrasonic oxidation of iodide was found to be significantly promoted by a small addition of CCl₄, and it was further found that the generation rate was increased with the amount of CCl₄ added. This can be used to analyze the level of CCl₄ dissolved in aqueous solutions. Under optimum conditions, the concentration of generated iodine (or its absorption at 351 nm) was found to correlated linearly with the concentration of CCl₄ in the range of 0.2-50 mg L⁻¹ (detection limit = 0.09 mg L⁻¹, R² = 0.999). As an alternative indirect spectrophotometric method of CCl₄ determination, the proposed method was successfully applied to determine the concentrations of CCl₄ in several practical samples, showing merits of being sensitive and simple of operation.