Rapid continuous microwave-assisted synthesis of silver nanoparticles to achieve very high productivity and full yield : from mechanistic study to optimal fabrication strategy

Systematic studies of silver nanoparticle synthesis in a continuous-flow single-mode microwave reactor using polyol process were performed, revealing that the synthesis is exceptionally effective to give very small metal particles at full reaction yield and very high productivity. Inlet concentration of silver nitrate or silver acetate, applied as metal precursors, varied between 10 and 50 mM, and flow rates ranged from 0.635 to 2.5 dm3/h, to give 3–24 s reaction time. Owing to its much higher reactivity, silver acetate was shown to be far superior substrate for the synthesis of small (10–20 nm) spherical silver nanoparticles within a few seconds. Its restricted solubility in ethylene glycol, applied as the solvent and reducing agent, appeared to be vital for effective separation of the stage of particle growth from its nucleation to enable rapid synthesis of small particles in a highly loaded system. This was not possible to obtain using silver nitrate. All the observations could perfectly be explained by a classical LaMer–Dinegar model of NPs’ formation, but taking into account also nonisothermal character of the continuous-flow process and acetate dissolution in the reaction system. The performed studies indicate an optimal strategy for the high-yield fabrication of metal particles using polyol method

Effect of ultrasonication time on microstructure, thermal conductivity, and viscosity of ionanofluids with originally ultra-long multi-walled carbon nanotubes

The stability along with thermal and rheological characteristics of ionanofluids (INFs) profoundly depend on the protocol of preparation. Therefore, in this work, the effect of ultrasonication time on microstructure, thermal conductivity, and viscosity of INFs containing 0.2 wt% of originally ultra-long multi-walled carbon nanotubes (MWCNTs) and four different ILs, namely 1-propyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide, 1- butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide, 1-ethyl-3-methylimidazolium thiocyanate, or 1- ethyl-3-methylimidazolium tricyanomethanide, was studied. The INFs were obtained by a two-step method using an ultrasonic probe. The ultrasonication process was performed for 1, 3, 10, or 30 min at a constant nominal power value of 200 W. The obtained results showed that for the shortest sonication time, the highest thermal conductivity enhancement of 12% was obtained. The extended sonication time from 1 to 30 min caused the cutting of MWCNTs and breaking the nanoparticle clusters, leading to a decrease in the average length of the nanotube bundles by approx. 70%. This resulted in a decline in thermal conductivity even by 7.2% and small deviations from the Newtonian behavior of INFs

Remarkable Thermal Conductivity Enhancement in Carbon-Based Ionanofluids: Effect of Nanoparticle Morphology

Transfer of the excellent intrinsic properties of individual carbon nanoparticles into real-life applications of the corresponding heat transfer fluids remains challenging. This process requires identification and quantification of the nanoparticle− liquid interface. Here, for the first time, we have determined geometry and properties of this interface by applying transmission electron cryomicroscopy (cryo-TEM). We have systematically investigated how the particle morphology of carbon-based nanomaterials affected the thermal conductivity, specific isobaric heat capacity, thermal diffusivity, density, and viscosity of ionanofluids and/or bucky gels, using a wide range of fillers, especially singlewalled carbon nanotubes (SWCNTs) and multiwalled carbon nanotubes (MWCNTs), both with extreme values of aspect ratio (length to diameter ratio) from 150 to 11 000. Accordingly, hybrid systems composed of various carbon nanomaterials and ionic liquid, namely 1-ethyl-3-methylimidazolium thiocyanate [EMIM][SCN], were prepared and characterized. Most of the analyzed nanodispersions exhibited long-term stability even without any surfactant. Our study revealed that the thermal conductivity could be remarkably improved to the maximum values of 43.9% and 67.8% for ionanofluid and bucky gel (at 1 wt % loadings of MWCNTs and SWCNTs), respectively, compared to the pristine ionic liquid. As a result, the model proposed by Murshed and co-workers has been improved for realistic description of the concentration-dependent thermal conductivity of such hybrid systems. The obtained results undoubtedly indicate the potential of ionanofluids and bucky gels for energy management

Thermophysical properties of IoNanofluids composed of 1-ethyl-3- methylimidazolium thiocyanate and carboxyl-functionalized long multi-walled carbon nanotubes

The concept of IoNanofluids (INFs) as the stable dispersions of nanoparticles in ionic liquids was proposed in 2009 by Nieto de Castro’s group. INFs characterize exciting properties such as improved thermal conductivity, non-volatility, and non-flammability. This work is a continuation of our studies on the morphology and physicochemistry of carbon-based nanomaterials a ecting thermal conductivity, viscosity, and density of INFs. We focus on the characterization of dispersions composed of long carboxylic group-functionalized multi-walled carbon nanotubes and 1-ethyl-3-methylimidazolium thiocyanate. The thermal conductivity of INFs was measured using KD2 Pro Thermal Properties Analyzer (Decagon Devices Inc., Pullman, WA, USA). The viscosity was investigated using rotary viscometer LV DV-II+Pro (Brookfield Engineering, Middleboro, MA, USA). The density of INFs was measured using a vibrating tube densimeter Anton Paar DMA 5000 (Graz, Austria). The maximum thermal conductivity enhancement of 22% was observed for INF composed of 1 wt% long carboxylic group-functionalized multi-walled carbon nanotubes

Rapid continuous microwave-assisted synthesis of silver nanoparticles to achieve very high productivity and full yield: from mechanistic study to optimal fabrication strategy

Systematic studies of silver nanoparticle synthesis in a continuous-flow single-mode microwave reactor using polyol process were performed, revealing that the synthesis is exceptionally effective to give very small metal particles at full reaction yield and very high productivity. Inlet concentration of silver nitrate or silver acetate, applied as metal precursors, varied between 10 and 50 mM, and flow rates ranged from 0.635 to 2.5 dm3/h, to give 3–24 s reaction time. Owing to its much higher reactivity, silver acetate was shown to be far superior substrate for the synthesis of small (10–20 nm) spherical silver nanoparticles within a few seconds. Its restricted solubility in ethylene glycol, applied as the solvent and reducing agent, appeared to be vital for effective separation of the stage of particle growth from its nucleation to enable rapid synthesis of small particles in a highly loaded system. This was not possible to obtain using silver nitrate. All the observations could perfectly be explained by a classical LaMer–Dinegar model of NPs’ formation, but taking into account also nonisothermal character of the continuous-flow process and acetate dissolution in the reaction system. The performed studies indicate an optimal strategy for the high-yield fabrication of metal particles using polyol method

Studies on the Preparation of Nanoparticles from Betulin-Based Polyanhydrides

Nanoparticles were obtained by nanoprecipitation and by emulsion solvent evaporation (ESE) method. In the ESE method, the size of the particles depended on the type and concentration of surfactant (in the water phase) and the polymer concentration (in the organic phase). The best results were obtained with ionic surfactants, however, the use of such compounds may accelerate the degradation process of polymers. In the nanoprecipitation method, the ratio of solvent (methylene chloride) to non-solvent (hexane) has a significant influence on the particle size. The smallest particles were obtained with a solvent to non-solvent ratio of 1:150

Application of Sonication and Microwave Irradiation to Boost Continuous Fabrication of the Copper(II) Oxide Sub-Micron Particles

Viability of the continuous-flow synthesis of rhomboidal copper(II) oxide (CuO) micro- and nanonoparticles was demonstrated. It has been shown that ultrasonic mixing of reactants, in the stage of Cu(OH)2 synthesis, followed by microwave irradiation of the resulting suspension, gives very fine particles of CuO at high yield and within minutes. Near optimal parameters for the synthesis of fine particles in the continuous reactor were determined

Hexokinase 2 inhibition and biological effects of BNBZ and its derivatives : the influence of the number and arrangement of hydroxyl groups

Hexokinase 2 (HK2), an enzyme of the sugar kinase family, plays a dual role in glucose metabolism and mediating cancer cell apoptosis, making it an attractive target for cancer therapy. While positive HK2 expression usually promotes cancer cells survival, silencing or inhibiting this enzyme has been found to improve the effectiveness of anti-cancer drugs and even result in cancer cell death. Previously, benitrobenrazide (BNBZ) was characterized as a potent HK2 inhibitor with good anti-cancer activity in mice, but the effect of its trihydroxy moiety (pyrogallol-like) on inhibitory activity and some cellular functions has not been fully understood. Therefore, the main goal of this study was to obtain the parent BNBZ (2a) and its three dihydroxy derivatives 2b–2d and to conduct additional physicochemical and biological investigations. The research hypothesis assumed that the HK2 inhibitory activity of the tested compounds depends on the number and location of hydroxyl groups in their chemical structure. Among many studies, the binding affinity to HK2 was determined and two human liver cancer cell lines, HepG2 and HUH7, were used and exposed to chemicals at various times: 24 h, 48 h and 72 h. The study showed that the modifications to the structures of the new BNBZ derivatives led to significant changes in their activities. It was also found that these compounds tend to aggregate and exhibit toxic effects. They were found to contribute to: (a) DNA damage, (b) increased ROS production, and (c) disruption of cell cycle progression. It was observed that, HepG2, occurred much more sensitive to the tested chemicals than the HUH7 cells; However, regardless of the used cell line it seems that the increase in the expression of HK2 in cancer cells compared to normal cells which have HK2 at a very low level, is a serious obstacle in anti-cancer therapy and efforts to find the effective inhibitors of this enzyme should be intensified

Biodegradable and Bioactive Carriers Based on Poly(betulin disuccinate-co-sebacic Acid) for Rifampicin Delivery

This paper describes the preparation and characterization of polymer-drug systems based on polymeric microspheres obtained from poly(betulin disuccinate-co-sebacic acid). The active compound that was coupled to the betulin-based carriers was rifampicin (RIF), an ansamycin drug used in the treatment of tuberculosis. Poly(betulin disuccinate-co-sebacic acid) microspheres were prepared using a solvent evaporation technique from copolymers obtained by polycondensation of betulin disuccinate (DBB) and sebacic acid (SEB). The content of sebacic acid in the copolymers was 20, 40, 60 and 80 wt%, respectively. Small and large rifampicin-loaded microspheres were obtained for each of the copolymers. The initial amount of drug was 10, 30 or 50 wt%, based on the weight of the polymer. Particles obtained in this study were round in shape with diameter in the range of 2–21 μm and of orange to red colour originating from rifampicin. The RIF encapsulation efficacy varied from 7% to 33%. Drug loading varied from 2% to 13% and increased at a higher RIF ratio. The highest degree of drug loading was observed for large particles, in which the initial amount of drug (at the particle preparation stage) was 50 wt%. Microspheres prepared from betulin-based polyanhydrides may have significant applications in drug delivery systems. The concentration of loaded drug was enough to obtain bactericidal effects against reference S. Aureus ATCC 25923 bacteria