Extraction of Cinnamomum longepaniculatum deciduous leaves essential oil using solvent-free microwave extraction: Process optimization and quality evaluation

The optimal process conditions for solvent-free microwave extraction(SFME)of essential oils from Cinnamomum longepaniculatum deciduous leaves after moisture conditioning were established by response surface methodology(RSM).A Box-Behnken design(BBD)was applied to evaluate the effects of three independent variables:moisture content(A:54%–74%),microwave power(B:300–500 W)and microwave time(C:20–40 min),on the extraction yield of essential oil.The compounds of the essential oils obtained by SFME,hydro-distillation and microwaveassisted hydro-distillation(MADE)were identified by gas chromatography-mass spectrometry(GC-MS),and the total lipids of C.longepaniculatum fresh leaves and deciduous leaves were analyzed.The correlation analysis of the response regression model indicated that quadratic polynomial model could be employed to optimize the extraction of essential oil.The optimal extraction condition was A:58%,B:400 W and C:28 min.In the optimal condition,the maximum extraction yield was 4.475 mL/100 g dw and higher than that by MADE.The main compound of the essential oil was eucalyptol(63.54%),and total oxygenated compounds was 78.95%,mainly caused by SFME and the metabolism of endophytic bacteria with decreasing content of phospholipids and fatty acids.Analysis of variance under the extraction condition illustrated high fitness of the model and the success of RSM for optimizing and reflecting the expected process condition.SFME combined with moisture regulation was an effective method for extracting essential oil from C.longepaniculatum deciduous leaves.

Solvent-free and catalyst-free method for the synthesis of 2,4,5-triarylimidazoles under microwave irradiation

A facile procedure for the synthesis of 2,4,5-lriarylimidazoles is being reported starting from benzil, aromatic aldehyde and ammonium acetate. The reactions were carried out with catalyst-free, solvent-free and under microwave irradiation conditions in high yield （80-99%） with short time （3-5 min） and environmental benign, as well as convenient operation. The structures of the compounds have been confirmed on the basis of their IR, 1H NMR, and/or 13C NMR, MS, and elemental analyzer.

Catalyst-free and solvent-free method for the synthesis of quinoxalines under microwave irradiation

A facile procedure for the synthesis, of quinoxalines is being reported starting from benzil and 1,2-diaminobenzene. The reactions were carried out catalyst-free, solvent-free and under microwave irradiation conditions in high yield （84-98%） with short time （3-6 min） and environmental benign, as well as convenient operation. The structures of all the compounds have been confirmed on the basis of their IR, 1H NMR, and/or 13C NMR, mass spectral data.

Solvent-Free Synthesis of Ultrafine Tungsten Carbide Nanoparticles-Decorated Carbon Nanosheets for Microwave Absorption

Carbides/carbon composites are emerging as a new kind of binary dielectric systems with good microwave absorption performance.Herein,we obtain a series of tungsten carbide/carbon composites through a simple solvent-free strategy,where the solid mixture of dicyandiamide(DCA)and ammonium metatungstate(AM)is employed as the precursor.Ultrafine cubic WC1-x nanoparticles(3-4 nm)are in situ generated and uniformly dispersed on carbon nanosheets.This configuration overcomes some disadvantages of conventional carbides/carbon composites and is greatly helpful for electromagnetic dissipation.It is found that the weight ratio of DCA to AM can regulate chemical composition of these composites,while less impact on the average size of WC1-x nanoparticles.With the increase in carbon nanosheets,the relative complex permittivity and dielectric loss ability are constantly enhanced through conductive loss and polarization relaxation.The different dielectric properties endow these composites with distinguishable attenuation ability and impedance matching.When DCA/AM weight ratio is 6.0,the optimized composite can produce good microwave absorption performance,whose strongest reflection loss intensity reaches up to-55.6 dB at 17.5 GHz and qualified absorption bandwidth covers 3.6-18.0 GHz by manipulating the thickness from 1.0 to 5.0 mm.Such a performance is superior to many conventional carbides/carbon composites.

Microwave-assisted synthesis of asymmetric thiocarbonohydrazones under solvent-free conditions

Six new asymmetric thiocarbonohydrazones 3a-3f were synthesized from following steps： firstly hydrazine hydrate reacted with carbon disulfide to form thiocarbonohydrazide （1） under microwave irradiation. Then compound （1） reacted with ketone and different aldehydes step by step to give 3a-3f with excellent yields under solvent-free conditions using microwave irradiation. Their structures have been determined by elemental analysis, IR, MS and ^1H NMR data. 2009 Qing Han Li. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All rights reserved.

An efficient and solvent-free one-pot synthesis of dihydropyrimidinones under microwave irradiation

An efficient synthesis of 3,4-dihydropyrimidin-2(1H)-one derivatives using formic acid as catalyst, from aldehydes, β-ketoester and urea(thiourea) without solvent under the irradiation of microwave is described. Compared with the classical Biginelli reaction, this new method has the advantage of good yields (77–94% for aromatic aldehydes) and short reaction time (3–8 min).

Microwave-assisted synthesis of new N^4-[bi-(4-fluorophenyl)-methyl]-piperazine thiosemicarbazones under solvent-free conditions

Six new N4-[bi-（4-fluorophenyl）-methyl]-piperazine thiosemicarbazones 3a-f have been prepared starting from [bi-（4-fluorophenyl）-methyl]-piperazine in solvent-free condition under microwave irradiation with excellent yields. Their structures have been determined by elemental analysis, IR, MS and 1H NMR data.

An expeditious and one-pot synthesis of unsymmetrical 2,5-disubstituted-1,3,4-oxadiazoles under microwave irradiation and solvent-free conditions

A one-pot synthesis of some unsymmetrical 2,5-disubstituted-1,3,4-oxadiazoles via cyclocondensation of benzoylhydrazines with orthoesters under solvent-free and microwave conditions are described here. The reaction is efficiently catalyzed by silica- supported sulfuric acid as it provided the title compounds in high yields and relatively short times. The catalyst is reusable and can be applied several times without considerable decrease in the yields and rates of the reactions.

A Rapid and Efficient Synthesis of Diaryl Thioureas via Solvent-Free Reaction Using Microwave

A rapid and efficient method for the preparation of diaryl thiourea compounds was reported for the first time. Twelve diaryl thiourea compounds that possessing biological activity have been synthesized in excellent yields (91-97%). The reaction proved to be extremely simple and highly efficient (in 1.5-4.5 min).

Antioxidant and Antimicrobial Activities of Essential Oils Extracted from Laurus nobilis L.Leaves by Using Solvent-Free Microwave and Hydrodistillation

In this study, laurel essential oils were obtained by using solvent-free microwave extraction (SFME) and hydrodistillation (HD) methods from Laurus nobilis leaves and determined their antioxidant and antimicrobial activity. Extraction time was reduced by about 43% in SFME at 622 W and 67% in SFME at 249 W compared to hydrodistillation. Essential oil of laurel was extracted by SFME at 622 W (100%) and 249 W (40%) power levels and HD inhibited oxidation generated by ABTS radical by 93.88%, 94.13% and 92.06%, respectively. Trolox equivalent antioxidant capacities (TEAC) of essential oils were 0.18 mM/mL oil for SFME at 622 W, 1.36 mM/mL oil for SFME at 249 W and 2.40 mM/mL oil for HD (p < 0.05). Essential oils of L. nobilis were extracted by SFME at 100% and 40% power levels and HD inhibited linoleic acid peroxidation by 70.57%, 63.53% and 89.18% respectively. Inhibition effects of laurel essential oils obtained by SFME at different power levels and HD on DPPH radical cation oxidation were not significantly different. The strongest antioxidant activity against DPPH radical was found in the essential oil obtained by SFME at 100% power level. Essential oils displayed antimicrobial activity against Staphylococcus aureus 6538P, Escherichia coli O157:H7 and Salmonella typhimurium NRRL E 4463 except for Listeria monocytogenes. The inhibitory effect on Staphylococcus aureus 6538P survival of laurel oil obtained from SFME by using lower power level was found to be lower than that obtained from SFME at 100% power level and HD

Microwave-promoted solvent-free synthesis of N-(diphenylmethylene)glycine alkyl esters

The efficient synthesis of N-（diphenylmethylene） glycine alkyl esters was achieved for the first microwave irradiation under solvent-free condition, using PEG or quaternary ammonium salts as phase transfer catalysts （PTCs）. Under the optimum conditions, N-（diphenylmethylene） glycine alkyl esters were obtained in excellent yields in most cases.

Catalyst and Solvent-Free Microwave Assisted Expeditious Synthesis of 3-Indolyl-3-hydroxy Oxindoles and Unsymmetrical 3,3-Di(indolyl)indolin-2-ones

A simple and efficient method for the synthesis of 3-indolyl-3-hydroxy oxindoles and unsymmetrical 3,3-di(indolyl)indolin-2-ones using microwave irradiation without catalyst and solvent is described. A series of 3-indolyl-3-hydroxy oxindoles and unsymmetrical 3,3-di(indolyl)indolin-2-ones have been synthesized in very short reaction times of 5 and 10 minutes and in yields ranging from 31% to 98% and from 53% to 78% respectively. This method offers a significant advantage over the conventional methods in terms of simplicity and shorter reaction time. To the best of our knowledge compounds N-allyl-3-hydroxy-3-(1-methyl-indol-3-yl)indolin-2-one (6c), N-allyl-3-hydroxy-3-(5-methoxy-indol-3-yl)indolin-2-one (8c), N-benzyl-3-hydroxy-3-(1-methyl-indol-3-yl) indolin-2-one (10c), N-propargyl-3-hydroxy-3-(1-methyl-indol-3-yl)indolin-2-one (13c), N-propargyl-3-hydroxy-3-(5-methoxy-indol-3-yl)indolin-2-one (14c), 3-(5-methoxy-1H-indol-3-yl)-3-(1H-indol-3-yl)indolin-2-one (1e), 3-1-methyl(5-methoxy-1H-indol-3-yl)-3-(1H-indol-3-yl)indolin-2-one (2e), 3-1-allyl(5-methoxy-1H-indol-3-yl)-3-(1H-indol-3-yl)indolin-2-one (3e), 3-1-benzyl(5-methoxy-1H-in- dol-3-yl)-3-(1H-indol-3-yl)indolin-2-one (4e) and 3-1-(prop-2-ynyl)(5-methoxy-1H-indol-3-yl)-3(1H-indol-3-yl)indolin-2-one (5e) are reported here for the first time. All the compounds are characterized by IR, 1H, 13C NMR and HRMS.

Microwave absorption and bandwidth study of Y_(2)Co_(17)rare earth soft magnetic alloy with easy-plane anisotropy

The easy-plane anisotropy of the Y_(2)Co_(17)rare earth soft magnetic alloy has high saturation magnetization and operating frequency,and good impedance matching.Therefore,it is expected to become a kind of high-performance microwave absorbing material.In this paper,Y_(2)Co_(17)alloy was prepared by a reduction-diffusion method,and its micropowder was prepared as polyurethane(PU)based composite absorbing materials(Y_(2)Co_(17)/PU composites).The microwave properties of composites with different volume fractions were calculated.The composites showed outstanding absorption characteristics in the range of 20-30 vol%,and the minimum reflection loss(RL)was less than-50 d B.When the volume fraction was25%,the effective absorption bandwidth could cover the X-band at a thickness of 1.5 mm,and the Ku-band at a thickness of1.08 mm.The absorption mechanism was analyzed by the interface reflection model.The RL absorption peak bandwidth mechanism was discussed by using the amplitude relation and calculating the effective absorption bandwidth at different thicknesses.The effective absorption bandwidth values were in good agreement with the theoretical expectation.

A TRUST REGION METHOD FOR MICROWAVE TOMOGRAPHY

A trust region method is proposed to solve the problem of microwave tomography,which is very difficult to be solved for its ill-posedness and nonlinearity. Compared with the Levenberg-Marquardt method, this method introduces more a priori knowledge and might obtain better results, though the two methods are equal in some cases.

The deconvolution of lunar brightness temperature based on the maximum entropy method using Chang'e-2 microwave data

A passive and multi-channel microwave sounder onboard the Chang＇e-2 orbiter has successfully acquired microwave observations of the lunar surface and subsurface structure. Compared with the Chang＇e-1 orbiter, the Chang＇e-2 orbiter obtained more accurate and comprehensive microwave brightness temperature data, which are helpful for further research. Since there is a close relationship between mi- crowave brightness temperature data and some related properties of the lunar regolith, such as the thickness, temperature and dielectric constant, precise and high resolution brightness temperature data are necessary for such research. However, through the detection mechanism of the microwave sounder, the brightness temperature data ac- quired from the microwave sounder are weighted by the antenna radiation pattern, so the data are the convolution of the antenna radiation pattern with the lunar brightness temperature. In order to obtain the real lunar brightness temperature, a deconvolution method is needed. The aim of this paper is to solve the problem associated with per- forming deconvolution of the lunar brightness temperature. In this study, we introduce the maximum entropy method （MEM） to process the brightness temperature data and achieve excellent results. The paper mainly includes the following aspects： first, we introduce the principle of the MEM; second, through a series of simulations, the MEM has been verified as an efficient deconvolution method; and third, the MEM is used to process the Chang＇e-2 microwave data and the results are significant.

Optimal Design of Aperture Illuminations for Microwave Power Transmission with Annular Collection Areas

This work presents an optimal design method of antenna aperture illumination for microwave power transmission with an annular collection area.The objective is to maximize the ratio of the power radiated on the annular collection area to the total transmitted power.By formulating the aperture amplitude distribution through a summation of a special set of series,the optimal design problem can be reduced to finding the maximum ratio of two real quadratic forms.Based on the theory of matrices,the solution to the formulated optimization problem is to determine the largest characteristic value and its associated characteristic vector.To meet security requirements,the peak radiation levels outside the receiving area are considered to be extra constraints.A hybrid grey wolf optimizer and Nelder–Mead simplex method is developed to deal with this constrained optimization problem.In order to demonstrate the effectiveness of the proposed method,numerical experiments on continuous apertures are conducted;then,discrete arrays of isotropic elements are employed to validate the correctness of the optimized results.Finally,patch arrays are adopted to further verify the validity of the proposed method.

High efficient oxygen reduction performance of Fe/Fe3C nanoparticles in situ encapsulated in nitrogen-doped carbon via a novel microwave-assisted carbon bath method

Fe-based carbon materials are widely considered promising to replace Pt/C as next-generation electrocatalysts towards oxygen reduction reaction (ORR). However, the preparation of Fe-based carbon materials is still carried out by conventional heating method (CHM). Herein, a novel microwave-assisted carbon bath method (MW-CBM) was proposed, which only took 35 min to synthesize Fe/Fe3C nanoparticles encapsulated in N-doped carbon layers derived from Prussian blue (PB). The catalyst contained large specific surface area and mesoporous structure, abundant Fe-Nx and C–N active sites, unique core-shell structure. Due to the synergistic effects of these features, the as-prepared Fe/Fe3C@NC-2 displayed outstanding ORR activity with onset potential of 0.98 VRHE and halfwave potential of 0.87 VRHE, which were more positive than 20 wt.% Pt/C (0.93 VRHE and 0.82 VRHE). Besides, Fe/Fe3C@NC-2 gave a better stability and methanol tolerance than Pt/C towards ORR in alkaline media, too.