Highly Efficient, One Pot Synthesis and Oxidation of Hantsch 1,4-Dihydropyridines Mediated by Iodobenzene Diacetate (III) Using Conventional Heating, Ultrasonic and Microwave Irradiation

A mild, general, convenient, and efficient one-pot synthesis of 4-arylpyridines (4) is described using conventional heating, ultrasound and microwave irradiation. Aryl aldehydes (2) were efficiently condensed with ethylacetoacetate (1) and ammonium acetate in acetonitrile to give dihydropyridine intermediates (4). The latter underwent a smooth Iodobenzene Diacetate (III) mediated aromatization reaction in the same pot to afford 4-arylpyridines (4) in good to excellent yields.

Effect of Combined Microwave-Ultrasonic Pretreatment on Anaerobic Biodegradability of Primary, Excess Activated and Mixed Sludge

This work deals with the effect of combined microwave-ultrasonic pretreatment on the anaerobic biodegradability of primary, excess activated and mixed sludge. The characteristics, biodegradability and anaerobic digester performance for untreated primary, excess activated and mixed sludge were compared to combined microwave-ultrasonic pretreated primary, excess activated and mixed sludge. All sludge samples were subjected to Microwave treatment at 2450 MHz, 800 W and 3 min followed by ultrasonic treatment at a density of 0.4 W/mL, amplitude of 90%, Intensity of 150 W, pulse of 55/5 for 6min. Methane production in pretreated primary sludge was significantly greater (11.9 ml/g TCOD) than the methane yield of the untreated primary sludge (7.9 ml/g TCOD). Cumulative methane production of pretreated Excess Activated Sludge (EAS) was higher (66.5 ml/g TCOD) than the methane yield from pretreated mixed sludge (44.1 ml/g TCOD). Furthermore, digested EAS showed significantly higher dewaterability (201 s) than digested primary sludge (305 s) or mixed sludge (522 s). The average Methane: Carbondioxide ratio from EAS (1.85) was higher than that for mixed untreated sludge (1.24). VS reduction was also higher for EAS than the other two sludge types. However, pretreatment of EAS resulted in significant reduction in dewaterability due to higher percentage of fine floc particles in the pretreated EAS.

Optimization of Process Parameters of Continuous Microwave Drying Raspberry Puree Based on RSM and ANN-GA

To improve drying uniformity and anthocyanin content of the raspberry puree dried in a continuous microwave dryer,the effects of process parameters(microwave intensity,air velocity,and drying time)on evaluation indexes(average temperature,average moisture content,average retention rate of the total anthocyanin content,temperature contrast value,and moisture dispersion value)were investigated via the response surface method(RSM)and the artificial neural network(ANN)with genetic algorithm(GA).The results showed that the microwave intensity and drying time dominated the changes of evaluation indexes.Overall,the ANN model was superior to the RSM model with better estimation ability,and higher drying uniformity and anthocyanin retention rate were achieved for the ANN-GA model compared with RSM.The optimal parameters were microwave intensity of 5.53 W•g^(-1),air velocity of 1.22 m·s^(-1),and drying time of 5.85 min.This study might provide guidance for process optimization of microwave drying berry fruits.

Evaluation of Improved Ultrasonic Nebulizer for Miniature Simultaneous Microwave Plasma Torch Spectrometer

A new automatic sample solution introduction system for miniature simultaneous microwave plasma torch（MPT） atomic emission spectrometer was developed. The operating parameters were optimized. The detection limits of the spectrometer with an ultrasonic nebulizer for Ag, Al, Ba, Ca, Cr, Cu, Fe, Mg, Mn, Sr, and V are 5-10 times lower than those obtained with a pneumatic nebulizer and are also lower than those obtained by a Model JX-lOlO MPT spectrometer. Two practical samples were analyzed to test the reliability and sensitivity of the system.

EVALUATON OF MICROWAVE PLASMA TORCH FOR ATOMIC FLUORESCENCE SPECTROMETRY WITH AN ULTRASONIC NEBULIZATION SAMPLE INTRODUCTION SYSTEM

In this paper, a new MPT(microwave plasma torch) device has been used as a atomizer for atomic fluorescence spectrometry. Spme elements, such as Zn, Cd, Hg, Pb, As, Co, Mg, Cu, Ag, Mn, Fe have been investigated in detail.

A Comparative Study of Process Parameter Optimization and Process of Flavonoid in Planted Trollius Chinensis through Backflow Method, Ultrasonic Wave Method and MicrowaveMethod

It takes flavonoid extraction rate as indicator and adopts the method of orthogonal experiment to study process of total flavonoid in Trollius chinensis through ultrasonic wave assisted extraction, microwave assisted extraction and backflow extraction, as well as optimization of process parameter. The result indicates that in terms of extraction efficiency, microwave extraction method is better than ultrasonic radiation extraction method, which is better than backflow extraction method. Optimal process parameter through backflow extraction is： backflow temperature 60℃, fluid material ratio 1：20, ethanol density 65%, backflow time 60min; optimal process parameter through ultrasonic wave assisted extraction is： ultrasonic radiation temperature 70℃, fluid material ratio 1：20, ethanol density 65%, ultrasonic wave radiation time 45rain; optimal process parameter of microwave assisted extraction is： microwave radiation temperature 60℃, fluid material ratio 1：20, ethanol density 75%, microwave radiation time 45min.

Ultrasonic Microwave Assisted Extraction of Polysaccharides from Sipunculus nudus

[Objectives] This study was conducted to optimize experimental conditions for extraction of polysaccharides from Sipunculus nudus.[Methods]With the Sipunculus nudus from Sanya as the experimental material,S.nudus polysaccharide was extracted by ultrasonic microwave assisted method,during which univariate factors including solid-liquid ratio,time,temperature,ultrasonic power,microwave power were investigated,to select optimal extracting conditions,which were also demonstrated and optimized by variance and response surface analysis.The optimized conditions were adopted to carry out a test,in which the absorbance of S.nudus polysaccharide was measured with an ultraviolet and visible spectrophotometer,followed by the calculation of the extracting amount of polysaccharide,and precision test and recovery test were also carried out to verify the experimental method.[Results]The standard solutions were determined at the maximum absorption wavelength of 486 nm,and the regression equation was A = 0.2677 C + 0.001 8,R^2= 0.999 8.Solid-liquid ratio,time,temperature,ultrasonic power and microwave power were investigated by univariate analysis and then optimized by response surface method as follows: solid-liquid ratio at 1:20( g/ml),time of 35 min,temperature at 50 ℃,ultrasonic power at 420 W and microwave power at 300 W,under which the measured extracting amount of S.nudus polysaccharide was1.37 mg/g.The RSD was 0.985% in precision experiment.In the repeatability test,the extracting amounts of polysaccharide were 1.41,1.43 and 1.38 mg/g for three parallel tests,respectively,with a RSD of 1.140%.The recovery test obtained following results: for group a( added with glucose standard) : the recovery of S.nudus polysaccharide was in the range of 100.3%-101.4%,RSD = 0.03%; and for group b( not added with glucose standard) : the recovery of S.nudus polysaccharide was in the range of 99.7%-100.3%,RSD = 0.02%.[Conclusions]The research method is stable and reliable.This study provides data basis and reference for follow-up study on S.nudus.

Synthesis of (Ca, Mg)-α′-Sialon-AlN-BN powders from boron-rich blast furnace slag by microwave carbothermal reduction-nitridation

(Ca, Mg)-α′-Sialon-AlN-BN powders were synthesized by the carbothermal reduction and nitridation (CRN) method using boron-rich slag, one of the intermediate products from pyrometallurgy separation of pageit, as the staring material. The influences of synthesis temperature and holding time on the phase composition and microstructure during the microwave CRN were studied by XRD, SEM and EDS. The comparison between two heating techniques, conventional and microwave heating, on the synthesized powder was presented as well. The experimental results revealed that the phase compositions and microstructures of the synthesized products were greatly affected by the synthesis temperature and holding time. With an increase in the synthesis temperature or holding time, the relative amount of α′-Sialon increased and α′-Sialon became the main crystalline phase at 1400 °C for 6 h. The synthesized products also contained AlN, BN and a small amount of β-SiC. Elongated α′-Sialon grains, short rod AlN grains, aggregate nanoscale BN grains were observed in the synthesized powders. The reaction temperature of microwave heating method was reduced by 80 °C, the reaction time was shortened by 2 h, and more elongated α′-Sialon grains with large aspect ratio were observed.

Superacid Catalyst SO4^2-/ZrO2-La2O3 Prepared by Ultrasonic Co-precipitation and Low Temperature Aging

Sulfated zirconia-lanthana （SO4^2-/ZrO2-La2O3） precursors were prepared by ultrasonic coprecipitation method and followed by aging at different temperature. The precursors were treated by 0.5 mol/L H2SO4. Samples of SO4^2-/ZrO2-La2O3 nano-crystalline catalysts were obtained by baking the treated precursors at different temperatures. The acidic properties of SO4^2-/ZrO2-La2O3 were tested by the Hammett indicator method. The phase composition, specific area, particle structure, and surface state were characterized by X-ray diffraction, BET, transmission electron microscopy, infrared spectrum, and X-ray photoelectron spec- troscopy. The catalytic activities were estimated by esterification of acetic acid with glycerin. It was shown that the catalyst prepared by ultrasonic stirring and low temperature （-15 ℃） exhibited highly active sites and high catalytic property.

超声波-微波联合辅助提取澳洲坚果青皮多糖工艺优化及其抗氧化活性

为了开发澳洲坚果青皮多糖产品,促进澳洲坚果青皮的综合利用,我们以澳洲坚果青皮为试材,比较澳洲坚果果实不同部位的多糖提取率,并采用超声波-微波联合辅助法,运用单因素与正交试验比较微波功率、提取时间、料液比、超声温度4个因素对多糖提取率的影响,研究其最优提取条件。以维生素C为对照,测定澳洲坚果青皮多糖清除1,1-二苯基-2-三硝基苯肼(DPPH)、羟基自由基的能力与还原力,评价其抗氧化活性。结果表明,澳洲坚果果实不同部位中,青皮多糖提取率最高。青皮多糖超声波-微波联合辅助提取工艺中各因素对提取率的影响力从高到低依次为提取时间>料液比>超声温度>微波功率,且均达到极显著水平(p<0.01),最佳提取工艺条件为提取时间90 min、超声温度65℃、料液比(1∶25)g/mL、微波功率400 W,此条件下提取率达到1.96%。澳洲坚果青皮多糖的抗氧化活性与质量浓度呈极显著正相关(p<0.01),相关系数R分别为0.9707、0.9813、0.9912,具有较强的DPPH、羟基自由基清除能力和较高的还原力,其半抑制浓度(IC 50)分别为38.55、20.38、41.51μg/mL,相同浓度下略低于维生素C。

The Optimization of Ultrasonic-assisted Extraction of Polysaccharide from Sipunculus nudus by Response Surface Methodology and Study on Antioxidant Activity

[Objectives]This study was conducted to optimize the extraction process of Sipunculus nudus polysaccharide and study the antioxidant activity of S. nudus polysaccharide. [Methods] S. nudus polysaccharide was extracted by ultrasonic microwave assisted method,during which univariate factors including solidliquid ratio,time,temperature,ultrasonic power,microwave power were investigated,to select optimal extracting conditions,which were also verified by an response surface optimization experiment( an four-factor three-level test); and the antioxidant activity of S. nudus polysaccharide was studied by determining its DPPH radical scavenging capacity. [Results]Through univariate factor investigation and response surface optimization test,it was found that the response surface results were consistent with univariate results. The optimized conditions were as follows: solid-liquid ratio at 1∶ 15,ultrasonic temperature at 60 ℃,ultrasonic power of 360 W and microwave power of 200 W,and the predicted polysaccharide extracting amount was 4. 35 mg/g. Under the optimized extracting conditions,the average extracting amount of S. nudus polysaccharide was 4. 38 mg/g,which is close to the theoretical predicted value( 4. 35 mg/g). And the results of this study also showed that different concentrations of polysaccharide solutions have different scavenging effects on DPPH free radical. At the polysaccharide concentration of0. 16 mg/ml,the maximum value of DPPH radical scavenging rate was 7. 22%,indicating that polysaccharide has certain antioxidant capacity. [Conclusions]This method is a new trial with satisfactory results.

Microstructure evolution and mechanical properties of the Sip/Zn- Al composite joints by ultrasonic-assisted soldering in air

Hypereutectic Al -27Si alloys were joined without flux by ultrasonic-assisted soldering at 420 ℃ in air using Zn -5Al the filler alloys, and Si particulate-reinforced Zn - Al based composites filler joints were obtained. The ultrasonic vibration introduced into soldering could influence the migration of Si particles and the microstructure of solidified Zn - Al based alloys. Both the distribution of Si particles and microstructure of the solidified Zn - Al based alloys affected the shear strength of joints. The shear strength increased with the ultrasonic vibration time. The highest average shear strength of joints reached to -68.5 MPa. Transcrystalline rupture mode was observed on the fracture surface.

Microwave-assisted Green and Efficient Synthesis of N^6-(2-Hydroxyethyl)adenosine and its Analogues

An efficient protocol for the synthesis of N^6-（2-Hydroxyethyl）adenosine and its analogues through nucleophilic substitution was developed. All the reactions were completed in 10 rain under microwave irradiation. Using water as solvent makes our method eco-friendly and easy to handle with.

Ultrasound-guided No Touch liver pedicle microwave ablation in hepatocellular carcinoma treatment

Objective This study aimed to investigate the feasibility,safety,and clinical effect of No Touch liver pedicle microwave ablation(NTLP-MWA).Methods The outcomes of 118 patients diagnosed with hepatocellular carcinoma(HCC)between 2014 and 2015 were retrospectively analyzed.Patients were divided into three groups.In group A,35 patients underwent ultrasound-guided NTLP-MWA,27 in Group B were treated with routine microwave ablation(RMWA),and 56 in group C underwent anatomic hepatectomy(AH).The preoperative basic data,intraoperative data,and postoperative data were analyzed among the three groups.Results The treatment time,intraoperative blood loss,and postoperative liver function(alanine transaminase)in the NTLP-MWA and RMWA groups were significantly different from those in the AH group(all P<0.005).There was no difference in the complete elimination rate and local recurrence within 1 year among the three groups.Treatment was not an independent risk factor for early postoperative recurrence.There was no significant difference in the 5-year overall survival rates among the three groups.Conclusion NTLP-MWA is safe and reliable,in accordance with the principles of oncology treatment,and worth further promotion in clinical practice.

Microwave promoted one-pot synthesis of 3-(2′-amino-3′-cyano-4′-arylpyrid-6′-yl)coumarins

A facile procedure for the synthesis of 3-（2′-amino-3′-cyano-4′-arylpyrid-6′-yl） coumarins are being reported starting from 3- acetylcoumarin, aromatic aldehydes and malononitrile. The reactions were carried out on microwave irradiation in good yield with short time and easy work-up. The structures of all the compounds have been confirmed on the basis of their analytical, IR, ^1H NMR, and mass spectral data.

Microwave absorption properties regulation and bandwidth formula of oriented Y_(2)Fe_(17)N_(3-δ)@SiO_(2)/PU composite synthesized by reduction-diffusion method

As concepts closely related to microwave absorption properties,impedance matching and phase matching were rarely combined with material parameters to regulate properties and explore related mechanisms.In this work,reduction–diffusion method was innovatively applied to synthesize rare earth alloy Y_(2)Fe_(17).In order to regulate the electromagnetic parameters of absorbers,the Y_(2)Fe_(17)N_(3-δ)particles were coated with silica(Y_(2)Fe_(17)N_(3-δ)@SiO_(2))and absorbers with different volume fractions were prepared.The relationship between impedance matching,matching thickness,and the strongest reflection loss peak(RLmin)was presented obviously.Compared to the microwave absorption properties of Y_(2)Fe_(17)N_(3-δ)/PU absorber,Y_(2)Fe_(17)N_(3-δ)@SiO_(2)/PU absorbers are more conducive to the realization of microwave absorption material standards which are thin thickness,light weight,strong absorbing intensity,and broad bandwidth.Based on microwave frequency bands,the microwave absorption properties of the absorbers were analyzed and the related parameters were listed.As an important parameter related to perfect matching,reflection factor(√ε_(r)/μ_(r))was discussed combined with microwave amplitude attenuation.According to the origin and mathematical model of bandwidth,the formula of EAB(RL<-10 dB)was derived and simplified.The calculated bandwidths agreed well with experimental results.

Microwave Synthesis and Crystal Structure of Bis{2-[(2,4-dichloro-phenylimino)methyl]-4,6-diiodo-phenol}-copper(Ⅱ)

Bis{2-[（2,4-dichloro-phenytimino）-methyl]-4,6-diiodo-phenol}-copper（II） （1） has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P21/n with a = 14.7558（17）, b = 20.770（2）, c = 20.3260（19） A, β = 90.6110（10）°, V= 6229.2（11） A3 and Z = 8. The Cu atom is surrounded by two O atoms and two N atoms from two 2-[（2,4-diehloro-phenylimino）-methyl]-4,6-diiodo-phenol molecules to form a tetrahedral coordination environment. The complex is linked into a column by weak intermolecular interactions.

Smart decontamination device for small-size radioactive scrap metal:using abrasion pin in rotating magnetic field and ultrasonic wave cleaner

A smart decontamination device is developed for small-size radioactive scrap metal(SSRSM)arisen from nuclear facilities.The abrasion pin in rotating magnetic field and ultrasonic wave cleaner are used for solving the problems of the second decontamination and high treatment cost.At first,the decontamination efficiency of each device is improved by upgrading the design.Optimal operating conditions are determined for each device.Next,both techniques are applied sequentially.Experimental results show that the efficiency of combined decontamination device is higher than that of each device.With the use of the developed device,the various SSRSMs are decontaminated for 15 min treatment in magnetic abrasion device and15 min treatment in ultrasonic cleaning device.Decontamination index ranges from18 to 56.Absolute values of all decontaminated samples are below the background value.

超声波-微波辅助双水相提取桑葚总黄酮工艺优化

以桑葚果实为原料,采用超声波-微波辅助乙醇-硫酸铵双水相提取总黄酮.采用单因素实验考察乙醇质量分数、硫酸铵质量分数、提取时间、微波功率、液料比等因素对总黄酮得率的影响,并以响应面分析法优化实验,确定总黄酮最佳提取工艺条件.实验结果表明:实验过程中超声波始终保持50 W,当乙醇质量分数为25%、硫酸铵质量分数为20%、提取时间为6.1 min、微波功率为300 W及液料比为27∶1(mL/g)时,桑葚中黄酮类化合物的提取得率最高,为17.44 mg/g.

铁皮石斛多糖超声-微波协同提取条件优化及其抗氧化活性

以铁皮石斛为原料,采用超声-微波协同法提取铁皮石斛多糖。选择液料比、微波时间、微波功率、超声时间为单因素,以铁皮石斛多糖提取率为评价指标,通过响应面试验对超声-微波协同法提取铁皮石斛多糖进行优化。确定最佳工艺参数为液料比50∶1(mL/g)、微波时间120 s、微波功率370 W、超声时间30 min,在此条件下铁皮石斛多糖提取率为30.56%。根据体外抗氧化活性评价表明,铁皮石斛多糖对羟自由基的清除能力低于维生素C,对α-葡萄糖苷酶表现出明显的抑制能力,具有较好的体外降血糖作用;另外,铁皮石斛多糖对α-淀粉酶也有一定的抑制作用。