Search Results (20)

Nanoparticle-catalysed microwave-aided multicomponent reactions (MCRs) have been demonstrated to be competent and environmentally benign tools for the quick synthesis of a wide spectrum of fused heterocyclic systems. The distinctive physicochemical properties of nanoparticles, including a substantial surface area, readily modifiable surface functionality, and heightened catalytic activities, when coupled with microwave irradiation, have enabled a marked improvement in reaction rates, product yields, and selectivity compared to conventional heating methods. This review highlights recent advancements in microwave-assisted MCRs facilitated by diverse nanomaterials, such as magnetic nanocatalysts, metal and metal oxide nanoparticles, mesoporous silica systems, and nanohybrids. It emphasises catalyst design, catalytic efficacy, scope, recyclability, and alignment with green chemistry principles in both solvent-free and aqueous environments, as well as the utilisation of recyclable catalysts. In summary, microwave-assisted multi-component reactions catalysed by nanoparticles are ecofriendly and versatile methods for the sustainable synthesis of such fused heterocycles containing bioactive pyridine, pyrazole, phenazine, pyrimidine, pyran, imidazole, and relevant pyridine derivatives, possessing potential in medicinal and material chemistry. Full article

A new composite microwave–dielectric system, (1 − x)Li_2.08TiO₃-xLi₂ZnTi₃O₈ (x = 0.3–0.7), was systematically investigated to identify the optimal composition for low-temperature co-fired ceramic (LTCC) applications by correlating sintering behavior, microstructural evolution, and microwave–dielectric properties. Although the undoped compositions exhibited excellent intrinsic dielectric performance, they required sintering at 1100 °C, making them incompatible with Ag-based LTCC processing. Among the investigated formulations, 0.6Li_2.08TiO₃–0.4Li₂ZnTi₃O₈ was identified as the most suitable base composition. To reduce the sintering temperature, 0.3–1.0 wt.% V₂O₅ was introduced as a sintering aid, enabling densification at 900 °C for 30 min (97.0% relative density) while preserving the coexistence of Li_2.08TiO₃ and Li₂ZnTi₃O₈ without XRD-detectable secondary phases. Microstructural observations indicated that V₂O₅ promoted liquid-phase sintering, leading to enhanced densification and Li_2.08TiO₃-selective abnormal grain coarsening without altering the intrinsic permittivity. Complementary dilatometry provided process-level evidence for this liquid-phase sintering mechanism: large total shrinkage at 900 °C ($∆L/L_o$≈ −17–19%), earlier ${\mathrm{T}}_{\mathrm{o}\mathrm{n}\mathrm{s}\mathrm{e}\mathrm{t}}$/${\mathrm{T}}_{\mathrm{p}\mathrm{e}\mathrm{a}\mathrm{k}}$ with ${\mathrm{T}}_{\mathrm{p}\mathrm{e}\mathrm{a}\mathrm{k}}$ lowered by ~250 °C, and an increased ${\mathrm{R}}_{\mathrm{p}\mathrm{e}\mathrm{a}\mathrm{k}}$, collectively supporting 900 °C/30 min as the practical firing window. The optimized 0.6Li_2.08TiO₃–0.4Li₂ZnTi₃O₈ composition containing 0.3 wt.% V₂O₅ exhibits excellent microwave–dielectric properties (${\epsilon }_{\mathit{r}}$ = 23.32, Q × f = 68,400 GHz, and ${\tau }_{\mathit{f}}$ = −1.55 ppm/°C). Higher V₂O₅ contents (>0.3 wt.%) caused a gradual reduction in Q × f due to increasing microstructural non-uniformity. Ag co-firing tests confirmed electrode stability with no interfacial reactions at 900 °C for 30 min. Overall, 0.3 wt.% V₂O₅-assisted 0.6Li_2.08TiO₃–0.4Li₂ZnTi₃O₈ provides a practical sub-950 °C processing window that satisfies key LTCC requirements, including moderate permittivity, high Q × f, near-zero ${\tau }_{\mathit{f}}$, and compatibility with Ag electrodes. Full article

The microwave-aided racemic synthesis of six 5-hydroxy-5-vinyl-2-cyclopentenone-type natural products was achieved. A key reaction involving the construction of the α-keto vinyl carbinol function was realized by applying a Mislow–Evans rearrangement of an allylic sulfoxide, which was prepared by conjugate addition of cyclopentane-1,3-dione-derived enolate to alkynyl sulfoxide to afford 5-hydroxy-3-methoxy-5-vinyl-2-cyclopentenone (1). From the common intermediate 1, five other congeneric natural products were synthesized. Full article

The banana weevil (Cosmopolites sordidus) is a significant pest that reduces banana yields and can result in plant mortality. (2R,5S)-theaspirane, a kairomone from senesced banana leaves, is one of the natural banana volatiles, aiding weevil attraction. A rapid and cost-effective synthesis of (2R,5S)-theaspirane was developed utilizing microwave-assisted conditions and the principles of green chemistry. The process comprised five steps, beginning with the reduction of dihydro-β-ionone, followed by lipase-mediated kinetic resolution to attain high enantiomeric excess. Microwave-assisted heating significantly reduced reaction times. Optimized cyclization with the minimum quantities of selenium dioxide oxidation was employed. The final diastereomers were separated by chromatography, yielding compounds which exceeded 99% enantiomeric purity. Full article

M²⁺N⁴⁺Nb₂O₈-type ceramics (where M = Mg, Ca, Mn, Co, Ni, Zn and N = Ti, Zr) are essential for satellite communication and mobile base stations due to their medium relative permittivity (ε_r) and high quality factor (Q × f). Although ZnTi_0.2Zr_0.8Nb₂O₈ ceramic exhibits impressive microwave dielectric properties, including an ε_r of 29.75, a Q × f of 107,303 GHz, and a τ_f of −24.41 ppm/°C, its sintering temperature of 1150 °C remains a significant barrier for integration into low-temperature co-fired ceramic (LTCC) technologies. To overcome this limitation, a strategy involving the partial substitution of Zn²⁺ with Cu²⁺ and the addition of LiF as a sintering aid was devised for ZnTi_0.2Zr_0.8Nb₂O₈. The dual impact of Cu²⁺ partial substitution and LiF as a sintering enhancer facilitated the successful sintering of Cu_0.3Zn_0.7Ti_0.2Zr_0.8Nb₂O₈ ceramics at a reduced temperature of 950 °C using the conventional solid-state reaction method. These ceramics exhibited excellent microwave dielectric properties. Notably, Cu_0.3Zn_0.7Ti_0.2Zr_0.8Nb₂O₈ ceramic with 40 mol% LiF addition demonstrated optimal microwave dielectric properties without any reaction with a silver electrode at a sintering temperature of 950 °C, yielding ε_r = 32, Q × f = 45,543 GHz, and τ_f = −43.5 ppm/°C. Full article

The depletion of fossil fuels, along with the environmental damages brought by their usage, calls for the development of a clean, sustainable and renewable source of energy. Biofuel, predominantly liquid biofuel such as biodiesel, is a promising alternative to fossil fuels, due to its compatible direct usage within the context of compression ignition engines. However, the industrial production of biodiesel is far from being energy and time efficient, which contributes to its high production cost. These inefficiencies are attributed to poor heat and mass transfer of the transesterification reaction. The utilisation of microchannel reactors is found to be excellent in escalating heat and mass transfer of the reactants, benefitting from their high surface area-to-volume ratio. The microchannel also intensifies the mixing of reactants via the reactor design, micromixers and the slug flow patterns within the reactor, thus enhancing the contact between reactants. Simulation studies have aided in the identification of mixing regimes within the microchannel reactors, induced by various reactor designs. In addition, microwave irradiation heating is found to enhance biodiesel production by localised superheating delivered directly to the reactants at a molecular level. This enables the reaction to begin much earlier, resulting in rapid biodiesel production. It is postulated that the synergy between microchannel reactors and microwave heating would catapult a pathway towards rapid and energy-efficient biodiesel production by enhancing heat and mass transfer between reactants. Full article

Designing efficient electrocatalytic systems through facile synthesis remains a formidable task. To address this issue, this paper presents the design of a combination material comprising two transition metal oxides (copper oxide and manganese oxide (CuO/MnO₂)), synthesized using a conventional microwave technique to efficiently engage as an active oxygen evolution reaction (OER) catalyst. The structural and morphological properties of the composite were confirmed by the aid of X-ray diffraction (XRD) studies, field emission scanning electron microscopy (FESEM), X-ray photoelectron spectroscopy (XPS), and energy-dispersive spectrometry (EDS). FESEM clearly indicated well-aligned interlacing of CuO with MnO₂. The OER performance was carried out in 1 M KOH. The assembled CuO/MnO₂ delivered a benchmark current density (j = 10 mA cm⁻²) at a minimal overpotential (η = 294 mV), while pristine CuO required a high η (316 mV). Additionally, the CuO/MnO₂ electrocatalyst exhibited stability for more than 15 h. These enhanced electrochemical performances were attributed to the large volume and expanded diameter of the pores, which offer ample surface area for catalytic reactions to boost OER. Furthermore, the rate kinetics of the OER are favored in composite due to low Tafel slope (77 mV/dec) compared to CuO (80 mV/dec). Full article

BaSi_xO_1+2x (1.61 ≤ x ≤ 1.90) and LiF-doped BaSi_1.63O_4.26 ceramics were prepared by using a traditional solid-state method at the optimal sintering temperatures. The evolution of phase compositions of BaSi_xO_1+2x (1.61 ≤ x ≤ 1.9) ceramics was revealed. The coexistence of Ba₅Si₈O₂₁ and Ba₃Si₅O₁₃ phases was obtained in BaSi_xO_1+2x (1.61 ≤ x ≤ 1.67) ceramics. The BaSi₂O₅ phase appeared inBaSi_xO_1+2x (1.68 ≤ x ≤ 1.90) ceramics. At 1.68 ≤ x ≤ 1.69, only BaSi₂O₅ and Ba₃Si₅O₁₃ phases existed. With the further increase in x, the Ba₅Si₈O₂₁ phase appeared, and BaSi₂O₅, Ba₅Si₈O₂₁ and Ba₃Si₅O₁₃ phases coexisted in BaSi_xO_1+2x (1.70 ≤ x ≤ 1.90) ceramics. The phase compositions of BaSi_xO_1+2x (1.61 ≤ x ≤ 1.90) ceramics were controlled by the ratio of Ba:Si. The BaSi_xO_1+2x (x = 1.68) ceramics with 98.15 wt% Ba₃Si₅O₁₃ and 1.85 wt% BaSi₂O₅ phases exhibited a negative τ_f value (−37.53 ppm/°C), and the good microwave dielectric properties of ε_r = 7.51, Q × f = 13,038 GHz and τ_f = +3.95 ppm/°C were obtained for BaSi_1.63O_4.26 ceramics with 70.05 wt% Ba₅Si₈O₂₁ and 29.95 wt% Ba₃Si₅O₁₃ phases. The addition of LiF sintering aids were able to reduce the sintering temperatures of BaSi_1.63O_4.26 ceramics to 800 °C. The phase composition of BaSi_1.63O_4.26 ceramics was affected by the sintering temperature, and the coexistence of Ba₅Si₈O₂₁, Ba₂Si₃O₈, BaSi₂O₅ and SiO₂ phases was achieved in BaSi_1.63O_4.26-3 wt% LiF ceramics. The BaSi_1.63O_4.26-3 wt% LiF ceramics sintered at 800 °C exhibited dense microstructures and excellent microwave dielectric properties (ε_r = 7.10, Q × f = 12,463 GHz and τ_f = +5.75 ppm/°C), and no chemical reaction occurred between BaSi_1.63O_4.26-3 wt% LiF ceramics and the Ag electrodes, which indicates their potential for low-temperature co-fired ceramic (LTCC) applications. Full article

Recognizing the extreme speeds of reactions with microwaves, anionic forms of surfactants (sodium dodecyl sulfate (SDS) and sodium dodecylbenzenesulfonate (SDBS)) have been intercalated successfully by ion-exchange reactions in binary Li-Al and ternary Li-M-Al (M = Mg, Co, Ni, Cu, and Zn) layered double hydroxide (LDH) systems with the aid of microwaves. The samples have been characterized extensively. The basal spacings of 28.2 and 30.4 Å have been estimated for Li-Al-DS and Li-Al-DBS LDH samples, respectively, suggesting a perpendicular arrangement of DS⁻ and DBS⁻ anions in the interlayer space. The characteristic vibration bands of both LDH and the surfactant (DS⁻ and DBS⁻) in the FTIR spectra confirmed the binding mode of surfactant molecules within the interlayers. DS⁻-intercalated Li-Al LDH showed lower thermal stability than the DBS⁻-intercalated sample. The nitrate-intercalated Li-M-Al (M = Mg, Co, Ni, Cu, and Zn) LDHs were ion-exchanged with SDS and SDBS to yield DS⁻-and DBS⁻-intercalated systems. The expanded basal spacings and a change in crystallite morphology confirmed the vertical intercalation of DS⁻ and DBS⁻ in Li-M-Al LDHs. ICP-AES and elemental analyses determined the metal contents and the surfactant content. FTIR spectra of intercalated samples confirmed the surfactant’s presence in the interlayer. The presence of Co, Ni, and Cu in Li-M-Al LDHs has been confirmed from UV-visible spectra. The Li-Al-DBS sample adsorbed iodine efficiently from methanol solutions, and the Langmuir model could explain the adsorption data in a better way. The adsorption followed pseudo-second-order kinetics. Full article

Organic peroxy radicals (RO₂) as key intermediates in tropospheric chemistry exert a controlling influence on the cycling of atmospheric reactive radicals and the production of secondary pollutants, such as ozone and secondary organic aerosols (SOA). Herein, we present a comprehensive study of the self-reaction of ethyl peroxy radicals (C₂H₅O₂) by using advanced vacuum ultraviolet (VUV) photoionization mass spectrometry in combination with theoretical calculations. A VUV discharge lamp in Hefei and synchrotron radiation at the Swiss Light Source (SLS) are employed as the photoionization light sources, combined with a microwave discharge fast flow reactor in Hefei and a laser photolysis reactor at the SLS. The dimeric product, C₂H₅OOC₂H₅, as well as other products, CH₃CHO, C₂H₅OH and C₂H₅O, formed from the self-reaction of C₂H₅O₂ are clearly observed in the photoionization mass spectra. Two kinds of kinetic experiments have been performed in Hefei by either changing the reaction time or the initial concentration of C₂H₅O₂ radicals to confirm the origins of the products and to validate the reaction mechanisms. Based on the fitting of the kinetic data with the theoretically calculated results and the peak area ratios in the photoionization mass spectra, a branching ratio of 10 ± 5% for the pathway leading to the dimeric product C₂H₅OOC₂H₅ is measured. In addition, the adiabatic ionization energy (AIE) of C₂H₅OOC₂H₅ is determined at 8.75 ± 0.05 eV in the photoionization spectrum with the aid of Franck-Condon calculations and its structure is revealed here for the first time. The potential energy surface of the C₂H₅O₂ self-reaction has also been theoretically calculated with a high-level of theory to understand the reaction processes in detail. This study provides a new insight into the direct measurement of the elusive dimeric product ROOR and demonstrates its non-negligible branching ratio in the self-reaction of small RO₂ radicals. Full article

Congo red (CR) is a stable anionic diazo dye that causes allergic reactions with carcinogenic properties. The rapid removal of CR using cation-incorporated nanohydroxyapatite (pristine HAp: X (X = Fe, Ni, Zn, Co, and Ag)) was investigated. The pristine and cation ion-doped HAp adsorbents were coprecipitated and subjected to hydrothermal and ultrasound treatments and subsequent microwave drying. The dopant ions significantly engineered the crystallite size, crystallinity, particle size (decreased 38–77%), shape (a rod to sphere modification by the incorporation of Ag⁺, Ni²⁺, and Co²⁺ ions), and colloidal stability (CS) of the adsorbent. These modifications aided in the rapid removal of the CR dye (98%) within one minute, and the CR adsorption rate was found to be significantly higher (93–99%) compared to previously reported rates. Furthermore, the kinetic, Langmuir, Freundlich, and DKR isotherms and thermodynamic results confirmed that the CR adsorption on the HAp was due to the strong chemical adsorption process. The order of the maximum CR adsorption capacity was Fe-HAp > HAp > Ag-HAp > Co-HAp > Zn-HAp. Whereas the CR regeneration efficiency was Fe-HAp (92%) > Ag-HAp (42%) > Ni-HAp (30%), with the other adsorbents exhibiting a poor recycling efficiency (1–16%). These results reveal Fe-HAp as a potential adsorbent for removing CR without the formation of byproducts. Full article

The use of thermal and non-thermal atmospheric pressure plasma to solve problems related to agriculture and biomedicine is the focus of this paper. Plasma in thermal equilibrium is used where heat is required. In agriculture, it is used to treat soil and land contaminated by the products of biomass, plastics, post-hospital and pharmaceutical waste combustion, and also by ecological phenomena that have recently been observed, such as droughts, floods and storms, leading to environmental pollution. In biomedical applications, thermal plasma is used in so-called indirect living tissue treatment. The sources of thermal plasma are arcs, plasma torches and microwave plasma reactors. In turn, atmospheric pressure cold (non-thermal) plasma is applied in agriculture and biomedicine where heat adversely affects technological processes. The thermodynamic imbalance of cold plasma makes it suitable for organic syntheses due its low power requirements and the possibility of conducting chemical reactions in gas at relatively low and close to ambient temperatures. It is also suitable in the treatment of living tissues and sterilisation of medical instruments made of materials that are non-resistant to high temperatures. Non-thermal and non-equilibrium discharges at atmospheric pressure that include dielectric barrier discharges (DBDs) and atmospheric pressure plasma jets (APPJs), as well as gliding arc (GAD), can be the source of cold plasma. This paper presents an overview of agriculture and soil protection problems and biomedical and health protection problems that can be solved with the aid of plasma produced with electrical discharges. In particular, agricultural processes related to water, sewage purification with ozone and with advanced oxidation processes, as well as those related to contaminated soil treatment and pest control, are presented. Among the biomedical applications of cold plasma, its antibacterial activity, wound healing, cancer treatment and dental problems are briefly discussed. Full article

In this work, spherical flower-shaped composite carbonyl iron powder@MnO₂ (CIP@MnO₂) with CIP as the core and ultrathin MnO₂ nanosheets as the shell was successfully prepared by a simple redox reaction to improve oxidation resistance and electromagnetic wave absorption properties. The microwave-absorbing properties of CIP@MnO₂ composites with different filling ratios (mass fractions of 20%, 40%, and 60% after mixing with paraffin) were tested and analyzed. The experimental results show that compared with pure CIP, the CIP@MnO₂ composites have smaller minimum reflection loss and a wider effective absorption bandwidth than CIP (RL < −20 dB). The sample filled with 40 wt% has the best comprehensive performance, the minimum reflection loss is −63.87 dB at 6.32 GHz, and the effective absorption bandwidth (RL < −20 dB) reaches 7.28 GHz in the range of 5.92 GHz–9.28 GHz and 11.2 GHz–15.12 GHz, which covers most C and X bands. Such excellent microwave absorption performance of the spherical flower-like CIP@MnO₂ composites is attributed to the combined effect of multiple beneficial components and the electromagnetic attenuation ability generated by the special spherical flower-like structure. Furthermore, this spherical flower-like core–shell shape aids in the creation of discontinuous networks, which improve microwave incidence dispersion, polarize more interfacial charges, and allow electromagnetic wave absorption. In theory, this research could lead to a simple and efficient process for producing spherical flower-shaped CIP@MnO₂ composites with high absorption, a wide band, and oxidation resistance for a wide range of applications. Full article

Uniform flowerlike microspheres Cd²⁺/Fe³⁺ co-doped BiOBr were prepared with the aid of the microwave hydrothermal process. The results indicate that the degradation performance of Bi_1−xCd_xOBr and Bi_1−xFe_xOBr are 1.31 and 2.05 times that of BiOBr for RhB, respectively. Moreover, the novel Cd²⁺/Fe³⁺ co-doped BiOBr photocatalysts with ~0.42 eV impurity bands presented remarkably enhanced photocatalytic activities with being 3.10 times that of pure BiOBr, by achieving e⁻/h⁺ efficient separation and narrowed bandgap with the ions synergistic effect of Cd²⁺ and Fe³⁺. Based on DFT insights, the photodegradation mechanism was systematically studied that the conversion of multivalent Fe³⁺ ions promoted the production of •O₂⁻, and Cd²⁺ ions worked as electron transfer mediators, which elucidated that the •O₂⁻ and h⁺_VB mainly participated in the catalytic reaction. The experimental and theoretical results show that the synergistic effects of multi-ion doping have great potential in the field of photocatalysis. Full article

A convenient and fast microwave synthesis of gold-doped titanium dioxide materials was developed with the aid of commercially available and common cyclodextrin derivatives, acting both as reducing and stabilizing agents. Anatase titanium oxide was synthesized from titanium chloride by microwave heating without calcination. Then, the resulting titanium oxide was decorated by gold nanoparticles thanks to a microwave-assisted reduction of HAuCl₄ by cyclodextrin in alkaline conditions. The materials were fully characterized by UV-Vis spectroscopy, X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM), and N₂ adsorption-desorption measurements, while the metal content was determined by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES). The efficiency of the TiO₂@Au materials was evaluated with respect to two different photocatalytic reactions, such as dye degradation and hydrogen evolution from water. Full article