Microwave-assisted Synthesis of Al_(4)SiC_(4) and Its Effect on Properties of MgO-C Refractories

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.

Mass-Based Environmental Factor and Energy Assessment of Microwave-Assisted Synthesized Transition Metal Nanostructures

This paper describes mass-based energy phase-space projection of microwave-assisted synthesis of transition metals (zinc oxide, palladium, silver, platinum, and gold) nanostructures. The projection uses process energy budget (measured in kJ) on the horizontal axes and process density (measured in kJg−1) on the vertical axes. These two axes allow both mass usage efficiency (Environmental-Factor) and energy efficiency to be evaluated for a range of microwave applicator and metal synthesis. The metrics are allied to the: second, sixth and eleventh principle of the twelve principle of Green Chemistry. This analytical approach to microwave synthesis (widely considered as a useful Green Chemistry energy source) allows a quantified dynamic environmental quotient to be given to renewable plant-based biomass associated with the reduction of the metal precursors. Thus allowing a degree of quantification of claimed “eco-friendly” and “sustainable” synthesis with regard to waste production and energy usage.

Microwave-Assisted Au and Ag Nanoparticle Synthesis: An Energy Phase-Space Projection Analysis

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-1) range between 180 ± 176.8 kJ, and 79.5 ± 79 kJ·ml-1, respectively. The axial field helical field an-tenna applicator is found to be the most energy efficient (0.253 kJ·m-1 per kJ, at 36 W). Followed by microwave ovens (4.47 ± 3.9 kJ·ml-1 per 76.83 ± 39 kJ), and TCMC ovens (2.86 ± 2.3 kJ·m-1 per 343 ± 321.5 kJ). The digester applicators have the least energy efficiency (36.2 ± 50.7 kJ·m-1 per 1010 ± 620 kJ). A comparison with reconstructed ‘non-thermal’ microwave oven inactivation microorganism experiments yields a power-law signature of n = 0.846 (R2 = 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.

Green Chemistry Allometry Test of Microwave-Assisted Synthesis of Transition Metal Nanostructures

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-1) 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.

Microwave-Assisted Transition Metal Nanostructure Synthesis: Power-Law Signature Verification

A power-law (y = cxn) signature between process energy budget (kJ) and process energy density (kJ·ml-1) 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-1. 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-1. 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-1 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.

Individualized Pixel Synthesis and Characterization of Combinatorial Materials Chips

Conventionally, an experimentally determined phase diagram requires studies of phase formation at a range of temperatures for each composition, which takes years of effort from multiple research groups. Combinatorial materials chip technology, featuring high-throughput synthesis and characterization, is able to determine the phase diagram of an entire composition spread of a binary or ternary system at a single temperature on one materials library, which, though significantly increasing efficiency, still requires many libraries processed at a series of temperatures in order to complete a phase diagram. In this paper, we propose a "one-chip method" to construct a complete phase diagram by individually synthesizing each pixel step by step with a progressive pulse of energy to heat at different temperatures while monitoring the phase evolution on the pixel in situ in real time. Repeating this process pixel by pixel throughout the whole chip allows the entire binary or ternary phase diagram to be mapped on one chip in a single experiment. The feasibility of this methodology is demonstrated in a study of a Ge-Sb-Te ternary alloy system, on which the amorphouscrystalline phase boundary is determined.

COMBINATORIAL SYNTHESIS OF MANNICH BASES IN SOLUTION/POLYMER REAGENT WORKUP

This paper describes a combinatorial Synthesis of the Mannich Bases in Solution through the Mannich reaction using 3 ketones, 5 amines and formaldehyde in solution and hydrochloride as a catalyst and then using a macroporous quarterized ammonium resin (CO32- form) as a scavenge agent to remove the acid catalyst when the Mannich reaction is completed. It was found by GC/MS analysis that the symmetrical ketone, such as acetone, in the Mannich reaction mainly produces one Mannich base; while the asymmetrical ketone, such as 2-pentanone, gives two Mannich bases. The reactivity depends on the tereo-hinder of both ketones and amines.

Microwave-assisted fast synthesis and red-emitting properties of a borotellurate-based phosphor with excellent thermostability

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.

Solvent- and catalyst-free synthesis of dihydropyrimidinthiones in one-pot under focused microwave irradiation conditions

Fifteen dihydropyrimidinthiones have been synthesized by microwave-assisted Biginelli reactions without any solvent or catalyst. The advantages of this novel protocol include the excellent yield, operational simplicity, short time and the avoidance of the use of organic solvents and catalysts.

The Microwave-assisted Preparation and X-Ray Structure of 3-Bromocarbazole-N-Acetic Acid

The rapid synthesis of 3-bromocarbarole-N-acetic acid was performed using microwave irradiation. Under the optimal conditions the yield was 85.6% . The crystal structure showed that the carboxylic groups form bifurcated hydrogen bonds and the hydroxyl oxygen atoms serve as proton donors and also acceptor. Each carboxylic group was involved in four hydrogen bonds. The package of crystal was dominated by links of these hydrogen bonds.

Facile Microwave-Assisted Synthesis of 2D Imine-Linked Covalent Organic Frameworks for Exceptional Iodine Capture

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.

Structure based library approach to photosynthesis inhibitors:Combinatorial synthesis of hydrouracil library

Based on the binding mode for hydrouracil in photosystem II (PS II) D1 protein, a general method for the solid phase combinatorial synthesis of hydrouracil library was developed. The acryloyl chloride or acid were coupled to Wang resin 1 to afford the acryloyl ester 2. Resin bound ester 2 reacted with various primary amines to give secondary amines 3, which were converted to the resin bound ureas 4 by treatment with isocyanates. Preparation of the hydrouracils 5 was achieved by the acidic cyclization_cleavage from the resin. For characterization purposes, 8 hydrouracil analogues were synthesized in parallel, following which a small library of 9 hydrouracil derivatives was prepared after cleavage from Wang resin. All the 9 bydrouracil derivatives desired were identified by GC_MS.

Microwave-assisted hydrothermal synthesis of copper oxide-based gas-sensitive nanostructures

Hydrothermal methods are widely used in chemical synthesis of target products with specific morphology and nanostructure.Those methods are very efficient for the preparation of well-controlled structures but the reaction time is usually long.The assistance of microwave makes the reaction system heat up faster,more uniformly and reactions are accelerated,it also can be utilized to change the morphology or structure of materials,which improves the physic-chemical properties of synthesized products and influences its gas-sensing performance.Copper oxide(CuO)is widely applied in semiconductor gas sensors because of its good reactivity and stability.This review article briefly introduces the principle,mechanism and recent development of CuO nanostructures obtained by microwave-as sis ted hydrothermal synthesis(MWHS)process.It also discussed the relation between endopathic factors of material and its gas-sensitive performance.The technical challenges and prospective solutions for highperformance CuO-based gas-sensitive materials with unique nanostructure are proposed.It is pointed out that the hierarchical CuO-based nanostructures and their composite materials prepared by MWHS process are efficacious methods to improve the gas-sensitive performance of the materials.On the basis of the morphology,the materials are divided into nanorods,nanoflowers,nanosheets,nanospheres and other nanostructures.The influence of microwave parameters on the properties of synthetic products is analyzed.The influence followed by metal element loading on the structure and properties of CuO-based materials by MWHS process is further discussed.Then this review summarizes the research progress of graphene-CuO and metal oxide-CuO composites prepared by MWHS process in recent years.

Microwave-assisted synthesis of some novel fluorinated pyrazolo[3,4-d]pyrimidine derivatives containing 1,3,4-thiadiazole as potential antitumor agents

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）.

Solvent-free microwave-assisted synthesis of tenorite nanoparticle-decorated multi-walled carbon nanotubes

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.

Microwave-assisted controllable synthesis of 2-acylbenzothiazoles and bibenzo[b][1,4]thiazines from aryl methyl ketones and disulfanediyldianilines

A condition-controlled strategy for selectively synthesis of 2-acylbenzothiazoles and bibenzo[b][1,4]thiazines from aryl methyl ketones and disulfanediyldianilines was realized using I_(2)/DMSO or I_(2)/MeCN systems,respectively.The desired products were synthesized in only 15 min with moderate to excellent yields(50%-90%)under microwave-assisted,metal-free conditions.The strategy provides a great advantage for selective synthetic applications in the efficient synthesis of benzothiazoles and bibenzothiazines heterocycle compounds.

Microwave-assisted synthesis and antimicrobial activities of 2-aryl-3-(naphthalene-1 or 2-yl)-1,3-thiazolidin-4-ones

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.