An optimized approach for the synthesis of N^1-ethoxymethyl-substituted cyclic inosine diphosphoribose（cIDPRE）,an analogue of cyclic adenosine diphosphoribose（cADPR）,has been developed via microwave-assisted intra...An optimized approach for the synthesis of N^1-ethoxymethyl-substituted cyclic inosine diphosphoribose（cIDPRE）,an analogue of cyclic adenosine diphosphoribose（cADPR）,has been developed via microwave-assisted intramolecular cyclization. The target compound has been successfully obtained through N^1-substitution,phosphorylation,cyclization and deprotection.By using this method,8-amino and bromo-substituted cIDPRE analogues were successfully obtained in good yield.The new approach has greatly shortened the synthetic route and enhanced the overall efficiency.展开更多
A facile microwave-assisted procedure for synthesis of novel fluorinated pyrazolo[3,4-d]pyrimidine derivatives containing 1,3,4-thiadiazole is described. This protocol presented such advantages as short reaction time,...A facile microwave-assisted procedure for synthesis of novel fluorinated pyrazolo[3,4-d]pyrimidine derivatives containing 1,3,4-thiadiazole is described. This protocol presented such advantages as short reaction time, high yields, simple purification and environmentally benign procedures. Their antitumor activities were evaluated against HL-60 by an MTT assay. The preliminary results indicated that some title compounds exhibit more potent antitumor inhibitory activity than doxorubicin （DOX）.展开更多
Al_(4)SiC_(4) was synthesized from Al powder, silicon carbide, and graphite by microwave sintering, and characterized by XRD and SEM. Then the synthesized material was added to the magnesia carbon refractory brick to ...Al_(4)SiC_(4) was synthesized from Al powder, silicon carbide, and graphite by microwave sintering, and characterized by XRD and SEM. Then the synthesized material was added to the magnesia carbon refractory brick to study its effect on the oxidation resistance, apparent porosity, bulk density, elastic modulus, and modulus of rupture. It is found that Al_(4)SiC_(4) can be synthesized by microwave sintering at 1 300 ℃ and the addition of Al_(4)SiC_(4)-containing material as an antioxidant can enhance the oxidation resistance of the magnesia carbon refractory brick.展开更多
Microwave irradiation is considered an important approach to Green Chemistry, because of its ability to rapidly increase the internal temperature of polar-organic compounds that lead to synthesis times of minutes rath...Microwave irradiation is considered an important approach to Green Chemistry, because of its ability to rapidly increase the internal temperature of polar-organic compounds that lead to synthesis times of minutes rather than hours when compared to conventional thermal heating. This works describes a dual allometry test for the discrimination between the solvents and reagents used in the microwave-assisted synthesis of transition metal (zinc oxide, palladium silver, platinum, and gold) nanostructures. The test is performed in log-log process energy phase-space projection, where the synthesis data (kJ against kJ·mol<sup>-1</sup>) has a power-law signature. The test is shown to discriminate between recommended Green Chemistry, problematic Green Chemistry, and Green Chemistry hazardous solvents. Typically, recommended Green chemistry exhibits a broad y-axes distribution within an upper exponent = 1 and lower exponent = 0.5. Problematic Green Chemistry exhibits a y-axes narrower distribution with an upper exponent = 0.94 and lower exponent = 0.64. Non-Green Chemistry hazardous data exhibits a further narrowing of the y-axes distribution within upper exponent = 0.87 and lower exponent = 0.66. In all three cases, the y-axes is aligned to original database power-law signature. It is also shown that in the x-axes direction (process energy budget) the grouped order of magnitude decreases from four orders for recommended Green Chemistry solvent and reagent data, through two orders for non-Green Chemistry hazardous material and down to one order for problematic Green Chemistry.展开更多
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 compo...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.展开更多
In this work, a fast(0.5 h), green microwave-assisted synthesis of single crystalline Sb_2Se_3 nanowires was developed. For the first time we demonstrated a facile solvent-mediated process, whereby intriguing nanostru...In this work, a fast(0.5 h), green microwave-assisted synthesis of single crystalline Sb_2Se_3 nanowires was developed. For the first time we demonstrated a facile solvent-mediated process, whereby intriguing nanostructures including antimony selenide(Sb_2Se_3) nanowires and selenium(Se) microrods can be achieved by merely varying the volume ratio of ethylene glycol(EG) and H_2O free from expensive chemical and additional surfactant. The achieved uniform Sb_2Se_3 nanowire is single crystalline along [001]growth direction with a diameter of 100 nm and a length up to tens of micrometers. When evaluated as an anode of lithium-ion battery, Sb_2Se_3 nanowire can deliver a high reversible capacity of 650.2 m Ah g^(-1) at 100 mA g^(-1) and a capacity retention of 63.8% after long-term 1000 cycles at 1000 mA g^(-1), as well as superior rate capability(389.5 m Ah g^(-1) at 2000 mA g^(-1)). This easy solvent-mediated microwave synthesis approach exhibits its great universe and importance towards the fabrication of high-performance metal chalcogenide electrode materials for future low-cost, large-scale energy storage systems.展开更多
An efficient synthesis of cinchona alkaloid-derived ligands based on solvent-free microwave-assisted reaction was described. The coupling of 1,4-dichlorophthalazine or 3,6-dichloropyridazine with quinine, cinchonine o...An efficient synthesis of cinchona alkaloid-derived ligands based on solvent-free microwave-assisted reaction was described. The coupling of 1,4-dichlorophthalazine or 3,6-dichloropyridazine with quinine, cinchonine or cinchonidine provide bis-or monocinchona alkaloid-derived ligands in moderate to good yields （52-89%） within 15 min under optimum microwave conditions.展开更多
Copper-decorated carbon nanotubes(CNTs) have important applications as precursors for ultraconductive copper wires. Tenorite-decorated CNTs(CuO-CNTs) are ideal candidates and are currently developed using laborious pr...Copper-decorated carbon nanotubes(CNTs) have important applications as precursors for ultraconductive copper wires. Tenorite-decorated CNTs(CuO-CNTs) are ideal candidates and are currently developed using laborious processes. For this reason, we have developed a facile and scalable method for the synthesis of CuO-CNTs from copper acetate. It was found that the optimal loading of copper acetate onto the CNTs was 23.1 wt% and that three 1-minute microwave treatments were sufficient for the decomposition of copper acetate to copper oxide. The loading of copper oxide onto the nanotubes was confirmed using X-ray photoelectron spectroscopy, energy-dispersive X-ray spectroscopy and thermogravimetric analysis. The materials were characterised using X-ray diffraction and scanning electron microscopy.展开更多
High density ZnO-nanorod arrays(rod length 1.59μm)were successfully synthesized via a microwave-assisted solution-phase method using zinc chloride and ammonia solution as reactants.The influence of concentration of a...High density ZnO-nanorod arrays(rod length 1.59μm)were successfully synthesized via a microwave-assisted solution-phase method using zinc chloride and ammonia solution as reactants.The influence of concentration of ammonia solution, work power,and microwave irradiation time on the morphology and size of final products was carefully investigated.The crystal structure,chemical composition and morphologies of final products were characterized using X-ray powder diffraction(XRD), scanning electron microscopy(SEM)and photoluminescence(PL).The as-synthesized ZnO is composed of single crystalline and possesses three photoluminescence emissions centered at 400,469 and 534.5 nm,respectively.展开更多
Li-argyrodites are promising solid electrolytes(SEs)for solid-state Li-ion batteries(SSLBs),but their large-scale industrial application remains a challenge.Conventional synthesis methods for SEs suffer from long reac...Li-argyrodites are promising solid electrolytes(SEs)for solid-state Li-ion batteries(SSLBs),but their large-scale industrial application remains a challenge.Conventional synthesis methods for SEs suffer from long reaction times and high energy consumption.In this study,we present a wet process for the synthesis of halogen-rich argyrodite Li_(6-a)PS_(5-a)Cl_(1+a)precursors(LPSCl_(1+a)-P,a=0–0.7)via an energysaving microwave-assisted process.Utilizing vibrational heating,we accelerate the formation of Liargyrodite precursor,even at excessive Cl-ion concentration,which significantly shortens the reaction time compared to traditional methods.After crystallization,we successfully synthesize the Liargyrodite,Li_(5.5)PS_(4.5)Cl_(1.5),which exhibits the superior ionic conductivity(7.8 mS cm^(-1))and low activation energy(0.23 eV)along with extremely low electric conductivity.The Li_(5.5)PS_(4.5)Cl_(1.5)exhibits superior Li compatibility owing to its high reversible striping/plating ability(over 5000 h)and high current density acceptability(1.3 mA cm^(-2)).It also exhibits excellent cycle reversibility and rate capability with NCM622 cathode(148.3 mA h g^(-1)at 1 C for 100 cycles with capacity retention of 85.6%).This finding suggests a potentially simpler and more scalable synthetic route to produce high-performance SEs.展开更多
Modifying the microstructure of photocatalysts while simultaneously introducing vacancies has shown significant potential in enhancing their performance for hydrogen production.Herein,a novel tubular mesoporous carbon...Modifying the microstructure of photocatalysts while simultaneously introducing vacancies has shown significant potential in enhancing their performance for hydrogen production.Herein,a novel tubular mesoporous carbon nitride(TMCN)with nitrogen vacancies was fabricated using a microwave-assisted synthesis strategy,employing melamine-cyanuric acid supramolecular(MC-S)as the precursor.The optimized TMCN exhibited an outstanding H_2 production rate,approximately 29 times higher than that of pristine g-C_(3)N_(4).The N-vacancies serve as sites for reactant adsorption and activation,leading to enhanced delocalization of HOMO-LUMO.Furthermore,the porous structures of TMCN facilitate the reactant diffusion,while its tubular architectures promote the oriented transfer of charge carriers.Crucially,the markedly improved photocatalytic performance of TMCN can be predominantly attributed to the synergistic effects arising from its superior structure and N-vacancy defects.This work opens new possibilities for the simultaneous formation of surface defect states as photocatalytic reaction sites and distinctive structures conducive to charge carrier transport.展开更多
Nanoscale europium（Ⅲ） metal-organic frameworks, Eu（BTC）（H20）.DMF, were synthesized by rapid microwave-assisted method. The components of the as-prepared products were confirmed by the elemental analysis, X-ray ...Nanoscale europium（Ⅲ） metal-organic frameworks, Eu（BTC）（H20）.DMF, were synthesized by rapid microwave-assisted method. The components of the as-prepared products were confirmed by the elemental analysis, X-ray powder diffraction （XRD）, thermal gravimetric analysis （TGA） and Fourier-transform infrared spectra （FTIR） analyses. Eu（BTC）（H20）.DMF with various morphologies, including particle-like, rod-like, straw-sheaf-like nanostructures, could be simply prepared by con- trolling the concentrations of the starting reactants. The optical measurements on the obtained Eu（BTC）（H20）- DMF indicated that all the nanomaterials show the characteristic emissions of the Eu3＋ ions at 578, 590, 612, 650, and 699 nm, which were at- tributed to 5Do→7FJ （J=0-4） transitions of the Eu3＋ ion, respectively. It was also noticed that the luminescent properties of the as-prepared products were heavily dependent on the morphologies and sizes of the nanomaterials. The assembled straw-sheaf-like architectures displayed the strongest emissions and the longest luminescence lifetime, which was mainly due to the fewest surface defects.展开更多
At present,with the increasing application needs of phosphor-converted white light-emitting diode(wLED),the synthetic efficiency and thermal stability of phosphor become urgent problems.Herein,this research reports a ...At present,with the increasing application needs of phosphor-converted white light-emitting diode(wLED),the synthetic efficiency and thermal stability of phosphor become urgent problems.Herein,this research reports a microwave-assisted fast synthesis approach to obtain a Sm^(3+)-activated borotellurate Na_(2)Y_(2)TeO_(4)(BO_(3))_(2)(NYTB)red phosphor with high crystallinity,excellent thermostability,and low chromaticity shift.For the NYTB-based phosphor,in contrast to the conventional solid-state synthesis,the microwave-assisted synthesis method involves lower synthesis temperature and shorter processing time.Additionally,the concentration quenching mechanism was determined.The w-LED device packaged with the studied phosphor exhibits a near-standard white light with proper CCT and high Ra parameters.展开更多
Covalent organic frameworks(COFs)have emerged as auspicious porous adsorbents for radioiodine capture.However,their conventional solvothermal synthesis demands multiday synthetic times and anaerobic conditions,largely...Covalent organic frameworks(COFs)have emerged as auspicious porous adsorbents for radioiodine capture.However,their conventional solvothermal synthesis demands multiday synthetic times and anaerobic conditions,largely hampering their practical use.To tackle these challenges,we present a facile microwave-assisted synthesis of 2D imine-linked COFs,Mw-TFB-BD-X,(X=−CH_(3) and−OCH_(3))under air within just 1 h.The resultant COFs possessed higher crystallinity,better yields,and more uniform morphology than their solvothermal counterparts.Remarkably,Mw-TFB-BD-CH_(3) and Mw-TFB-BDOCH_(3) exhibited exceptional iodine adsorption capacities of 7.83 g g^(−1) and 7.05 g g^(−1),respectively,placing them among the bestperforming COF adsorbents for static iodine vapor capture.Moreover,Mw-TFB-BD-CH_(3) and Mw-TFB-BD-OCH_(3) can be reused 5 times with no apparent loss in the adsorption capacity.The exceptionally high iodine adsorption capacities and excellent reusability of COFs were mainly attributed to their uniform spherical morphology and enhanced chemical stability due to the in-built electron-donating groups,despite their low surface areas.This work establishes a benchmark for developing advanced iodine adsorbents that combine fast kinetics,high capacity,excellent reusability,and facile rapid synthesis,a set of appealing features that remain challenging to merge in COF adsorbents so far.展开更多
Three-dimensional flowerlike α-Ni（OH）2 nanostructures were successfully synthesized by the microwave-assisted reflux as short as 30 rain. The crystalline structure and morphology of the products were characterized ...Three-dimensional flowerlike α-Ni（OH）2 nanostructures were successfully synthesized by the microwave-assisted reflux as short as 30 rain. The crystalline structure and morphology of the products were characterized by X-ray diffraction, N2 adsorption-desorption isotherms, field emission scanning electron microscopy, and transmission electron microscopy. The α-Ni（OH）2 nanostructure shows a large surface area of 173 m2 g-1 and narrow mesopore distribution. The electrochemical properties of the as-prepared α-Ni（OH）2 as an electrode material for supercapacitor were investigated by cyclic voltammetry and galvanostatic charge-discharge measurements in 6 mol/L KOH electrolyte. The α-Ni（OH）2 nanostructure shows a maximum specific capacitance of 2030 F g-1 at a current density of 1 A g-1 and exhibits excellent rate capability. These results suggest that it is a promising electrode material for supercapacitor application.展开更多
2-aryl-3-(naphthalene-1 or 2-yl)-1,3-thiazolidin-4-ones 4 and 5 were synthesized in 41%–67%yield by using microwave-assisted one-pot protocol.The structures of the new compounds 4l,4m,5c,5e,5g,5h,and 5j–5m were conf...2-aryl-3-(naphthalene-1 or 2-yl)-1,3-thiazolidin-4-ones 4 and 5 were synthesized in 41%–67%yield by using microwave-assisted one-pot protocol.The structures of the new compounds 4l,4m,5c,5e,5g,5h,and 5j–5m were confirmed by IR,NMR,MS,and elemental analysis.The antimicrobial activities of the compounds against Pseudomonas syringae pv.lachrymans(Smith et Bryan)Young,Dye&Wilkie,Botrytis cinerea Pers.,and Sphaerotheca fusca Blum.were examined.Some of the compounds showed good antifungical activity against Sphaerotheca fusca Blum.展开更多
Agreen regioselective synthesis of some new and known 9-aryl-5,9-dihydropyrimido[4,5-d][l,2,4]triazolo[1,5-a]pyrimidine-6,8（4H,7H）-diones has been described via the microwave-assisted one-pot reaction of 3-amino-1H-...Agreen regioselective synthesis of some new and known 9-aryl-5,9-dihydropyrimido[4,5-d][l,2,4]triazolo[1,5-a]pyrimidine-6,8（4H,7H）-diones has been described via the microwave-assisted one-pot reaction of 3-amino-1H-1,2,4-triazoles,aromatic aldehydes and barbituric acids under solvent- and catalyst-free conditions.This operationally simple procedure is less laborious and provides a better scope than previously reported procedures.展开更多
A power-law (y = cx<sup>n</sup>) signature between process energy budget (kJ) and process energy density (kJ·ml<sup>-1</sup>) of microwave-assisted synthesis of silver and gold nanostructu...A power-law (y = cx<sup>n</sup>) signature between process energy budget (kJ) and process energy density (kJ·ml<sup>-1</sup>) of microwave-assisted synthesis of silver and gold nanostructures has been recently described [Law and Denis. AJAC, 14(4), 149-174, (2023)]. This study explores this relation further for palladium, platinum, and zinc oxide nanostructures. Parametric cluster analysis and statistical analysis is used to test the power-law signature of over four orders of magnitude as a function of six microwave applicator-types metal precursor, non-Green Chemistry synthesis and claimed Green Chemistry. It is found that for the claimed Green Chemistry, process energy budget ranges from 0.291 to 900 kJ, with a residual error ranging between −33 to +25.9 kJ·ml<sup>-1</sup>. The non-Green Chemistry synthesis has a higher process energy budget range from 3.2 kJ to 3.3 MJ, with a residual error of −33.3 to +245.3 kJ·ml<sup>-1</sup>. It is also found that the energy profile over time produced by software controlled digestion applicators is poorly reported which leads to residual error problematic outliers that produce possible phase-transition in the power-law signature. The original Au and Ag database and new Pd, Pt and ZnO database (with and without problematic outliers) yield a global microwave-assisted synthesis power-law signature constants of c = 0.7172 ± 0.3214 kJ·ml<sup>-1</sup> at x-axes = 0.001 kJ, and the exponent, n = 0.791 ± 0.055. The information in this study is aimed to understand variations in historical microwave-assisted synthesis processes, and develop new scale-out synthesis through process intensification.展开更多
Microwave-assisted synthesis of gold and silver nanoparticles, as a function of Green Chemistry, non Green Chemistry, and four applicator types are reported. The applicator types are Domestic microwave ovens, commerci...Microwave-assisted synthesis of gold and silver nanoparticles, as a function of Green Chemistry, non Green Chemistry, and four applicator types are reported. The applicator types are Domestic microwave ovens, commercial temperature controlled microwave chemistry ovens (TCMC), digesters, and axial field helical antennae. For each of these microwave applicators the process energy budget where estimated (Watts multiplied by process time = kJ) and energy density (applied energy divided by suspension volume = kJ·ml<sup>-1</sup>) range between 180 ± 176.8 kJ, and 79.5 ± 79 kJ·ml<sup>-1</sup>, respectively. The axial field helical field an-tenna applicator is found to be the most energy efficient (0.253 kJ·m<sup>-1</sup> per kJ, at 36 W). Followed by microwave ovens (4.47 ± 3.9 kJ·ml<sup>-1</sup> per 76.83 ± 39 kJ), and TCMC ovens (2.86 ± 2.3 kJ·m<sup>-1</sup> per 343 ± 321.5 kJ). The digester applicators have the least energy efficiency (36.2 ± 50.7 kJ·m<sup>-1</sup> per 1010 ± 620 kJ). A comparison with reconstructed ‘non-thermal’ microwave oven inactivation microorganism experiments yields a power-law signature of n = 0.846 (R<sup>2</sup> = 0.7923) four orders of magnitude. The paper provides a discussion on the Au and Ag nanoparticle chemistry and bio-chemistry synthesis aspects of the microwave applicator energy datasets and variation within each dataset. The visual and analytical approach within the energy phase-space projection enables a nanoparticle synthesis route to be systematically characterized, and where changes to the synthesis are to be mapped and compared directly with historical datasets. In order to help identify lower cost nanoparticle synthesis, in addition to potentially reduce synthesis energy to routes informed changes to potentially reduce synthesis energy budget, along with nanoparticle morphology and yield.展开更多
Among various architectures of polymers,end-group-free rings have attracted growing interests due to their distinct physicochemical performances over the linear counterparts which are exemplified by reduced hydrodynam...Among various architectures of polymers,end-group-free rings have attracted growing interests due to their distinct physicochemical performances over the linear counterparts which are exemplified by reduced hydrodynamic size and slower degradation.It is key to develop facile methods to large-scale synthesis of polymer rings with tunable compositions and microstructures.Recent progresses in large-scale synthesis of polymer rings against single-chain dynamic nanoparticles,and the example applications in synchronous enhancing toughness and strength of polymer nanocomposites are summarized.Once there is the breakthrough in rational design and effective large-scale synthesis of polymer rings and their functional derivatives,a family of cyclic functional hybrids would be available,thus providing a new paradigm in developing polymer science and engineering.展开更多
基金National Natural Science Foundation of China (Grant No.20910094) Ministry of Education of China(Grant No.200800010078)
文摘An optimized approach for the synthesis of N^1-ethoxymethyl-substituted cyclic inosine diphosphoribose（cIDPRE）,an analogue of cyclic adenosine diphosphoribose（cADPR）,has been developed via microwave-assisted intramolecular cyclization. The target compound has been successfully obtained through N^1-substitution,phosphorylation,cyclization and deprotection.By using this method,8-amino and bromo-substituted cIDPRE analogues were successfully obtained in good yield.The new approach has greatly shortened the synthetic route and enhanced the overall efficiency.
基金the National Nature Science Foundation of Hubei Province(No.2008CDB016)the Scientific Research Fund of Hubei Provincial Education Department(No.D20111904)
文摘A facile microwave-assisted procedure for synthesis of novel fluorinated pyrazolo[3,4-d]pyrimidine derivatives containing 1,3,4-thiadiazole is described. This protocol presented such advantages as short reaction time, high yields, simple purification and environmentally benign procedures. Their antitumor activities were evaluated against HL-60 by an MTT assay. The preliminary results indicated that some title compounds exhibit more potent antitumor inhibitory activity than doxorubicin （DOX）.
基金This work was funded by Luoyang Major Science and Technology Innovation Project(2301009A)Henan Province Key Research and Development Project(231111230200)。
文摘Al_(4)SiC_(4) was synthesized from Al powder, silicon carbide, and graphite by microwave sintering, and characterized by XRD and SEM. Then the synthesized material was added to the magnesia carbon refractory brick to study its effect on the oxidation resistance, apparent porosity, bulk density, elastic modulus, and modulus of rupture. It is found that Al_(4)SiC_(4) can be synthesized by microwave sintering at 1 300 ℃ and the addition of Al_(4)SiC_(4)-containing material as an antioxidant can enhance the oxidation resistance of the magnesia carbon refractory brick.
文摘Microwave irradiation is considered an important approach to Green Chemistry, because of its ability to rapidly increase the internal temperature of polar-organic compounds that lead to synthesis times of minutes rather than hours when compared to conventional thermal heating. This works describes a dual allometry test for the discrimination between the solvents and reagents used in the microwave-assisted synthesis of transition metal (zinc oxide, palladium silver, platinum, and gold) nanostructures. The test is performed in log-log process energy phase-space projection, where the synthesis data (kJ against kJ·mol<sup>-1</sup>) has a power-law signature. The test is shown to discriminate between recommended Green Chemistry, problematic Green Chemistry, and Green Chemistry hazardous solvents. Typically, recommended Green chemistry exhibits a broad y-axes distribution within an upper exponent = 1 and lower exponent = 0.5. Problematic Green Chemistry exhibits a y-axes narrower distribution with an upper exponent = 0.94 and lower exponent = 0.64. Non-Green Chemistry hazardous data exhibits a further narrowing of the y-axes distribution within upper exponent = 0.87 and lower exponent = 0.66. In all three cases, the y-axes is aligned to original database power-law signature. It is also shown that in the x-axes direction (process energy budget) the grouped order of magnitude decreases from four orders for recommended Green Chemistry solvent and reagent data, through two orders for non-Green Chemistry hazardous material and down to one order for problematic Green Chemistry.
基金the Natural Science Foundation of Southwest University for Nationalities (No.08NQZ002) for financial support.
文摘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.
基金supported by the National Key Research and Development Program of China(2016YFA0202603)the National Basic Research Program of China(2013CB934103)+5 种基金the National Natural Science Foundation of China(51521001,51602239)the National Natural Science Fund for Distinguished Young Scholars(51425204)Yellow Crane Talent(Science&Technology)Program of Wuhan Citythe Fundamental Research Funds for the Central Universities(WUT:2016III001,2016III003,2016IVA090)the Programme of Introducing Talents of Discipline to Universities(B17034)support from the Lorraine Region(nowpart of Grand Est Region)Cooperation Research Lorraine/Hubei Program 2015/2017
文摘In this work, a fast(0.5 h), green microwave-assisted synthesis of single crystalline Sb_2Se_3 nanowires was developed. For the first time we demonstrated a facile solvent-mediated process, whereby intriguing nanostructures including antimony selenide(Sb_2Se_3) nanowires and selenium(Se) microrods can be achieved by merely varying the volume ratio of ethylene glycol(EG) and H_2O free from expensive chemical and additional surfactant. The achieved uniform Sb_2Se_3 nanowire is single crystalline along [001]growth direction with a diameter of 100 nm and a length up to tens of micrometers. When evaluated as an anode of lithium-ion battery, Sb_2Se_3 nanowire can deliver a high reversible capacity of 650.2 m Ah g^(-1) at 100 mA g^(-1) and a capacity retention of 63.8% after long-term 1000 cycles at 1000 mA g^(-1), as well as superior rate capability(389.5 m Ah g^(-1) at 2000 mA g^(-1)). This easy solvent-mediated microwave synthesis approach exhibits its great universe and importance towards the fabrication of high-performance metal chalcogenide electrode materials for future low-cost, large-scale energy storage systems.
基金the National Natural Science Foundation of China (No.20672141) for financial support of this work.
文摘An efficient synthesis of cinchona alkaloid-derived ligands based on solvent-free microwave-assisted reaction was described. The coupling of 1,4-dichlorophthalazine or 3,6-dichloropyridazine with quinine, cinchonine or cinchonidine provide bis-or monocinchona alkaloid-derived ligands in moderate to good yields （52-89%） within 15 min under optimum microwave conditions.
基金the financial support provided by the Welsh Government Sêr Cymru National Research Network in Advanced Engineering and Materials (NRN-150)the Sêr Cymru Chair Programme (A.R.B.)+8 种基金the Sêr Cymru II Fellowship (C.E.G.)the Sêr Cymru II Recapturing Talent Fellowship (E.K.)partly funded by the European Regional Development Fund (ERDF)part of the Flexible Integrated Energy Systems (FLEXIS) and Reducing Industrial Carbon Emissions (RICE) research operations funded by the Welsh European Funding Office (WEFO)provided by the Engineering and Physical Sciences Research Council (EPSRC) UK, the Robert A. Welch Foundation (C-0002)King Saud Universitythe assistance provided by the Swansea University AIM Facility, which was funded in part by the EPSRC (EP/M028267/1)the European Regional Development Fund through the Welsh Government (80708)the Sêr Solar project via the Welsh Government
文摘Copper-decorated carbon nanotubes(CNTs) have important applications as precursors for ultraconductive copper wires. Tenorite-decorated CNTs(CuO-CNTs) are ideal candidates and are currently developed using laborious processes. For this reason, we have developed a facile and scalable method for the synthesis of CuO-CNTs from copper acetate. It was found that the optimal loading of copper acetate onto the CNTs was 23.1 wt% and that three 1-minute microwave treatments were sufficient for the decomposition of copper acetate to copper oxide. The loading of copper oxide onto the nanotubes was confirmed using X-ray photoelectron spectroscopy, energy-dispersive X-ray spectroscopy and thermogravimetric analysis. The materials were characterised using X-ray diffraction and scanning electron microscopy.
基金Project supported by the Postdoctoral Science Foundation of Central South University,ChinaProjects(50621063,30700008)supported by the National Natural Science Foundation of China
文摘High density ZnO-nanorod arrays(rod length 1.59μm)were successfully synthesized via a microwave-assisted solution-phase method using zinc chloride and ammonia solution as reactants.The influence of concentration of ammonia solution, work power,and microwave irradiation time on the morphology and size of final products was carefully investigated.The crystal structure,chemical composition and morphologies of final products were characterized using X-ray powder diffraction(XRD), scanning electron microscopy(SEM)and photoluminescence(PL).The as-synthesized ZnO is composed of single crystalline and possesses three photoluminescence emissions centered at 400,469 and 534.5 nm,respectively.
基金supported by the Basic Science Research Program through National Research Foundation of Korea(NRF)grant funded by the Ministry of Science and ICT(RS-2022-NR070534)supported by the National Research Council of Science&Technology(NST)grant by the Korea government(MSIT)(2710024139)。
文摘Li-argyrodites are promising solid electrolytes(SEs)for solid-state Li-ion batteries(SSLBs),but their large-scale industrial application remains a challenge.Conventional synthesis methods for SEs suffer from long reaction times and high energy consumption.In this study,we present a wet process for the synthesis of halogen-rich argyrodite Li_(6-a)PS_(5-a)Cl_(1+a)precursors(LPSCl_(1+a)-P,a=0–0.7)via an energysaving microwave-assisted process.Utilizing vibrational heating,we accelerate the formation of Liargyrodite precursor,even at excessive Cl-ion concentration,which significantly shortens the reaction time compared to traditional methods.After crystallization,we successfully synthesize the Liargyrodite,Li_(5.5)PS_(4.5)Cl_(1.5),which exhibits the superior ionic conductivity(7.8 mS cm^(-1))and low activation energy(0.23 eV)along with extremely low electric conductivity.The Li_(5.5)PS_(4.5)Cl_(1.5)exhibits superior Li compatibility owing to its high reversible striping/plating ability(over 5000 h)and high current density acceptability(1.3 mA cm^(-2)).It also exhibits excellent cycle reversibility and rate capability with NCM622 cathode(148.3 mA h g^(-1)at 1 C for 100 cycles with capacity retention of 85.6%).This finding suggests a potentially simpler and more scalable synthetic route to produce high-performance SEs.
基金supported by the National Natural Science Foundation of China (22369024)。
文摘Modifying the microstructure of photocatalysts while simultaneously introducing vacancies has shown significant potential in enhancing their performance for hydrogen production.Herein,a novel tubular mesoporous carbon nitride(TMCN)with nitrogen vacancies was fabricated using a microwave-assisted synthesis strategy,employing melamine-cyanuric acid supramolecular(MC-S)as the precursor.The optimized TMCN exhibited an outstanding H_2 production rate,approximately 29 times higher than that of pristine g-C_(3)N_(4).The N-vacancies serve as sites for reactant adsorption and activation,leading to enhanced delocalization of HOMO-LUMO.Furthermore,the porous structures of TMCN facilitate the reactant diffusion,while its tubular architectures promote the oriented transfer of charge carriers.Crucially,the markedly improved photocatalytic performance of TMCN can be predominantly attributed to the synergistic effects arising from its superior structure and N-vacancy defects.This work opens new possibilities for the simultaneous formation of surface defect states as photocatalytic reaction sites and distinctive structures conducive to charge carrier transport.
基金supported by the National Natural Science Foundation of China(21101148,21371165,51372242,21210001,21471144)the National Natural Science Foundation for Creative Research Group(21221061)Jilin Province Youth Foundation(201201005,201201008)
文摘Nanoscale europium（Ⅲ） metal-organic frameworks, Eu（BTC）（H20）.DMF, were synthesized by rapid microwave-assisted method. The components of the as-prepared products were confirmed by the elemental analysis, X-ray powder diffraction （XRD）, thermal gravimetric analysis （TGA） and Fourier-transform infrared spectra （FTIR） analyses. Eu（BTC）（H20）.DMF with various morphologies, including particle-like, rod-like, straw-sheaf-like nanostructures, could be simply prepared by con- trolling the concentrations of the starting reactants. The optical measurements on the obtained Eu（BTC）（H20）- DMF indicated that all the nanomaterials show the characteristic emissions of the Eu3＋ ions at 578, 590, 612, 650, and 699 nm, which were at- tributed to 5Do→7FJ （J=0-4） transitions of the Eu3＋ ion, respectively. It was also noticed that the luminescent properties of the as-prepared products were heavily dependent on the morphologies and sizes of the nanomaterials. The assembled straw-sheaf-like architectures displayed the strongest emissions and the longest luminescence lifetime, which was mainly due to the fewest surface defects.
基金Project supported by the National Natural Science Foundation of China(22165031,21761034)NationalUndergraduate Innovation and Entrepreneurship Foundation(202210673034)Scientific Research Foundation of Education Departmentof Yunnan province(2022Y001)。
文摘At present,with the increasing application needs of phosphor-converted white light-emitting diode(wLED),the synthetic efficiency and thermal stability of phosphor become urgent problems.Herein,this research reports a microwave-assisted fast synthesis approach to obtain a Sm^(3+)-activated borotellurate Na_(2)Y_(2)TeO_(4)(BO_(3))_(2)(NYTB)red phosphor with high crystallinity,excellent thermostability,and low chromaticity shift.For the NYTB-based phosphor,in contrast to the conventional solid-state synthesis,the microwave-assisted synthesis method involves lower synthesis temperature and shorter processing time.Additionally,the concentration quenching mechanism was determined.The w-LED device packaged with the studied phosphor exhibits a near-standard white light with proper CCT and high Ra parameters.
基金supported by the U.S.Department of Energy Office of Science Early Career Research Program(DESC0022000)the National Science Foundation HBCU-UPRIA program(no.2100360)+2 种基金the U.S.Department of Defense,the Office of Naval Research(no:N00014-20-1-2523)supported by the Office of Science,Office of Basic Energy Sciences,of the U.S.Department of Energy under Contract No.DE-AC02-05CH11231the support from Qassim University.S.C.is grateful for the support from the National Natural Science Foundation of China(no.22171092).
文摘Covalent organic frameworks(COFs)have emerged as auspicious porous adsorbents for radioiodine capture.However,their conventional solvothermal synthesis demands multiday synthetic times and anaerobic conditions,largely hampering their practical use.To tackle these challenges,we present a facile microwave-assisted synthesis of 2D imine-linked COFs,Mw-TFB-BD-X,(X=−CH_(3) and−OCH_(3))under air within just 1 h.The resultant COFs possessed higher crystallinity,better yields,and more uniform morphology than their solvothermal counterparts.Remarkably,Mw-TFB-BD-CH_(3) and Mw-TFB-BDOCH_(3) exhibited exceptional iodine adsorption capacities of 7.83 g g^(−1) and 7.05 g g^(−1),respectively,placing them among the bestperforming COF adsorbents for static iodine vapor capture.Moreover,Mw-TFB-BD-CH_(3) and Mw-TFB-BD-OCH_(3) can be reused 5 times with no apparent loss in the adsorption capacity.The exceptionally high iodine adsorption capacities and excellent reusability of COFs were mainly attributed to their uniform spherical morphology and enhanced chemical stability due to the in-built electron-donating groups,despite their low surface areas.This work establishes a benchmark for developing advanced iodine adsorbents that combine fast kinetics,high capacity,excellent reusability,and facile rapid synthesis,a set of appealing features that remain challenging to merge in COF adsorbents so far.
基金supported by the National Natural Science Foundation of China(Grant No.51472238)the Open Project Program of State Key Laboratory of Chemical Resource Engineering(Grant No.CRE-2014-C-102)
文摘Three-dimensional flowerlike α-Ni（OH）2 nanostructures were successfully synthesized by the microwave-assisted reflux as short as 30 rain. The crystalline structure and morphology of the products were characterized by X-ray diffraction, N2 adsorption-desorption isotherms, field emission scanning electron microscopy, and transmission electron microscopy. The α-Ni（OH）2 nanostructure shows a large surface area of 173 m2 g-1 and narrow mesopore distribution. The electrochemical properties of the as-prepared α-Ni（OH）2 as an electrode material for supercapacitor were investigated by cyclic voltammetry and galvanostatic charge-discharge measurements in 6 mol/L KOH electrolyte. The α-Ni（OH）2 nanostructure shows a maximum specific capacitance of 2030 F g-1 at a current density of 1 A g-1 and exhibits excellent rate capability. These results suggest that it is a promising electrode material for supercapacitor application.
基金The financial supports from the National Natural Science Foundation of China(Grant No.20672027)the Natural Science Foundation of Hebei(2005000106,2008000588)+1 种基金the Research Foundation of the Ministry of Education of China(206013)the Postdoctoral Foundation of China are gratefully acknowledged.
文摘2-aryl-3-(naphthalene-1 or 2-yl)-1,3-thiazolidin-4-ones 4 and 5 were synthesized in 41%–67%yield by using microwave-assisted one-pot protocol.The structures of the new compounds 4l,4m,5c,5e,5g,5h,and 5j–5m were confirmed by IR,NMR,MS,and elemental analysis.The antimicrobial activities of the compounds against Pseudomonas syringae pv.lachrymans(Smith et Bryan)Young,Dye&Wilkie,Botrytis cinerea Pers.,and Sphaerotheca fusca Blum.were examined.Some of the compounds showed good antifungical activity against Sphaerotheca fusca Blum.
文摘Agreen regioselective synthesis of some new and known 9-aryl-5,9-dihydropyrimido[4,5-d][l,2,4]triazolo[1,5-a]pyrimidine-6,8（4H,7H）-diones has been described via the microwave-assisted one-pot reaction of 3-amino-1H-1,2,4-triazoles,aromatic aldehydes and barbituric acids under solvent- and catalyst-free conditions.This operationally simple procedure is less laborious and provides a better scope than previously reported procedures.
文摘A power-law (y = cx<sup>n</sup>) signature between process energy budget (kJ) and process energy density (kJ·ml<sup>-1</sup>) of microwave-assisted synthesis of silver and gold nanostructures has been recently described [Law and Denis. AJAC, 14(4), 149-174, (2023)]. This study explores this relation further for palladium, platinum, and zinc oxide nanostructures. Parametric cluster analysis and statistical analysis is used to test the power-law signature of over four orders of magnitude as a function of six microwave applicator-types metal precursor, non-Green Chemistry synthesis and claimed Green Chemistry. It is found that for the claimed Green Chemistry, process energy budget ranges from 0.291 to 900 kJ, with a residual error ranging between −33 to +25.9 kJ·ml<sup>-1</sup>. The non-Green Chemistry synthesis has a higher process energy budget range from 3.2 kJ to 3.3 MJ, with a residual error of −33.3 to +245.3 kJ·ml<sup>-1</sup>. It is also found that the energy profile over time produced by software controlled digestion applicators is poorly reported which leads to residual error problematic outliers that produce possible phase-transition in the power-law signature. The original Au and Ag database and new Pd, Pt and ZnO database (with and without problematic outliers) yield a global microwave-assisted synthesis power-law signature constants of c = 0.7172 ± 0.3214 kJ·ml<sup>-1</sup> at x-axes = 0.001 kJ, and the exponent, n = 0.791 ± 0.055. The information in this study is aimed to understand variations in historical microwave-assisted synthesis processes, and develop new scale-out synthesis through process intensification.
文摘Microwave-assisted synthesis of gold and silver nanoparticles, as a function of Green Chemistry, non Green Chemistry, and four applicator types are reported. The applicator types are Domestic microwave ovens, commercial temperature controlled microwave chemistry ovens (TCMC), digesters, and axial field helical antennae. For each of these microwave applicators the process energy budget where estimated (Watts multiplied by process time = kJ) and energy density (applied energy divided by suspension volume = kJ·ml<sup>-1</sup>) range between 180 ± 176.8 kJ, and 79.5 ± 79 kJ·ml<sup>-1</sup>, respectively. The axial field helical field an-tenna applicator is found to be the most energy efficient (0.253 kJ·m<sup>-1</sup> per kJ, at 36 W). Followed by microwave ovens (4.47 ± 3.9 kJ·ml<sup>-1</sup> per 76.83 ± 39 kJ), and TCMC ovens (2.86 ± 2.3 kJ·m<sup>-1</sup> per 343 ± 321.5 kJ). The digester applicators have the least energy efficiency (36.2 ± 50.7 kJ·m<sup>-1</sup> per 1010 ± 620 kJ). A comparison with reconstructed ‘non-thermal’ microwave oven inactivation microorganism experiments yields a power-law signature of n = 0.846 (R<sup>2</sup> = 0.7923) four orders of magnitude. The paper provides a discussion on the Au and Ag nanoparticle chemistry and bio-chemistry synthesis aspects of the microwave applicator energy datasets and variation within each dataset. The visual and analytical approach within the energy phase-space projection enables a nanoparticle synthesis route to be systematically characterized, and where changes to the synthesis are to be mapped and compared directly with historical datasets. In order to help identify lower cost nanoparticle synthesis, in addition to potentially reduce synthesis energy to routes informed changes to potentially reduce synthesis energy budget, along with nanoparticle morphology and yield.
基金Supported by the National Natural Science Foundation of China(Nos.52293472,22473096 and 22471164)。
文摘Among various architectures of polymers,end-group-free rings have attracted growing interests due to their distinct physicochemical performances over the linear counterparts which are exemplified by reduced hydrodynamic size and slower degradation.It is key to develop facile methods to large-scale synthesis of polymer rings with tunable compositions and microstructures.Recent progresses in large-scale synthesis of polymer rings against single-chain dynamic nanoparticles,and the example applications in synchronous enhancing toughness and strength of polymer nanocomposites are summarized.Once there is the breakthrough in rational design and effective large-scale synthesis of polymer rings and their functional derivatives,a family of cyclic functional hybrids would be available,thus providing a new paradigm in developing polymer science and engineering.
