Phase change materials (PCMs) are used for latent heat storage. Most promising applications of PCMs are waste heat recovery systems, solar heating systems, building energy conservation systems, and air-conditioning systems. Macroporous poly(ethylene dimethacrylate) (PEDMA) carrier beads were formed by the suspension polymerization technique, imbibed with paraffin or cetyl alcohol phase change materials and coated with a silica shell to prevent their aggregation and the leakage of PCM. PEDMA beads contained 75.6 % paraffin and 53.1 % cetyl alcohol resulting in high latent heat storage capacities. The melting and crystallizing enthalpies were 132.6 and 133.4 J/g, respectively for paraffin-loaded capsules, while 89.6 and 88.6 J/g, respectively for cetyl alcohol containing beads. The excellent latent heat storage of the capsules was retained after 1,000 heating-cooling cycles indicating that the capillary forces of the silicacoated porous polymer beads efficiently prevented the leakage of the PCMs.
We have developed a simple method to prepare nano-(ZrC0.93, ZrO2-polymorphs)@carbon composites with graphite/amorphous carbon content and adjustable Zr/C ratio based on using a multistep tube furnace and plasma-assisted heat treatment of zirconium-loaded sulfonated styrene–divinylbenzene (STY-DVB) copolymers. Pre-pyrolysis of zirconium-loaded sulfonated STY-DVB ion exchangers with 2 and 8 mass % DVB at temperatures between 1000 and 1400 °C for 2 h produced nano-ZrO2@C intermediates with particle sizes of ~ 30–60 nm with no ZrC formation. Plasma processing of nano-ZrO2@C resulted in nano-(ZrC0.93, ZrO2)@C composites with 11% (under a He atmosphere) (C/Zr = 73) or 13% (under a H2 atmosphere) (C/Zr = 58) ZrC0.93 content. Three polymorphs of the zirconium dioxide (tetragonal, monoclinic and cubic, between 18 and 27 nm) were found in the products. The amounts of tetragonal and monoclinic ones are comparable to that of ZrC0.93. The average particle size of ZrC0.93 prepared in this way was found to be 21–23 nm. The BET surface area of the nano-(ZrC0.93, ZrO2)@C(graphite) composites prepared in He and H2 was over 250 and 300 m2/g, respectively. We developed a reproducible and easy method to prepare nano-(ZrC, ZrO2)@C products by setting the DVB content, sulfonation degree, Zr loading and the thermal treatment conditions, which have an influence on the ZrC and graphite/amorphous carbon content of nano-ZrO2@C intermediates. The zirconium-loaded sulfonated styrene–divinylbenzene (STY-DVB) copolymers (2 and 8 mass% DVB) or their thermal decomposition was characterized with vibrational spectroscopy, thermal analysis and DSC or powder XRD, BET, XPS and HRTEM methods, respectively.
Latent heat storing calcium alginate microcapsules were manufactured by a repeated interfacial coacervation/crosslinking method. By using a high-viscosity sodium alginate for the capsule formation, the paraffin phase change material (PCM) content was substantially enhanced related to the recently developed procedure. The maximization of PCM loading was achieved using experimental design for paraffin containing microcapsules. The microcomposites were optimized for 81.5 % PCM content with uniform size of 2.20 ± 0.14 mm. In some applications e.g. packaging, the biodegradable character of the materials is especially beneficial, hence for the manufacture of entirely eco-friendly heat storing microcomposites coconut oil PCM was microencapsulated by the same procedure. The process originally developed and optimized for paraffin was scaled-up by two orders of magnitude, accordingly, the outstanding PCM content was reproduced also with coconut oil (average value 81.1 %). The high PCM content was reflected also in the heat storing capacity measured by differential scanning calorimetry. The easily upscalable, spherical and core/shell structured, entirely biocompatible microcapsules with thermally stable calcium alginate coating could be developed for industrial application.
Microencapsulation of phase change materials (PCMs) is an attractive opportunity for broadening their applications. In this respect, a novel encapsulating polymer, ethyl cellulose (EC) was used to entrap n-hexadecane (HD) PCM by an emulsion-solvent evaporation method. Emulsifiers strongly influenced the size and morphology of the forming EC-HD composite microcapsules, and they also had a great impact on their thermal properties. All of the three emulsifiers were suitable to prepare quasi core-shell microparticles, though the high porosity of shells resulted in serious leakage in composites prepared by Tween 80, and permeability of particles manufactured by poly(vinyl alcohol) (PVA), as can be stated from scanning electron microscopy and differential scanning calorimetry analysis. Interfacial tension measurements and spreading coefficient analysis enabled the prediction of preparation conditions for usable core-shell microcapsules. Volume weighted mean diameters of the microparticles were 319 m, 92 m and 85 m formed by Tween 80, PVA and poly(methacrylic acid sodium salt) (PMAA), repectively. A significantly higher HD content and latent heat storage capacity could be achieved using PVA and PMAA than with Tween 80. The thermal cycling test indicated good thermal reliability of microcapsules prepared by PMAA, while the energy-storing capacity of composites prepared by PVA decreased substantially, and a dramatic reduction was found in microparticles using Tween 80.
Dual drug-loaded nanotherapeutics can play an important role against the drug resistance and side effects of the single drugs. Doxorubicin and sorafenib were efficiently co-encapsulated by tailor-made poly([R,S]-3-hydroxybutyrate) (PHB) using an emulsion–solvent evaporation method. Subsequent poly(ethylene glycol) (PEG) conjugation onto nanoparticles was applied to make the nanocarriers stealth and to improve their drug release characteristics. Monodisperse PHB–sorafenib–doxorubicin nanoparticles had an average size of 199.3 nm, which was increased to 250.5 nm after PEGylation. The nanoparticle yield and encapsulation efficiencies of drugs decreased slightly in consequence of PEG conjugation. The drug release of the doxorubicin was beneficial, since it was liberated faster in a tumor-specific acidic environment than in blood plasma. The PEG attachment decelerated the release of both the doxorubicin and the sorafenib, however, the release of the latter drug remained still significantly faster with increased initial burst compared to doxorubicin. Nevertheless, the PEG–PHB copolymer showed more beneficial drug release kinetics in vitro in comparison with our recently developed PEGylated poly(lactic-co-glycolic acid) nanoparticles loaded with the same drugs.
In this study, relationships between preparation conditions, structure, and activity of Pt-containing TiO2 photocatalysts in photoinduced reforming of glycerol for H2 production were explored. Commercial Aerolyst® TiO2 (P25) and homemade TiO2 prepared by precipitation-aging method were used as semiconductors. Pt co-catalysts were prepared by incipient wetness impregnation from aqueous solution of Pt(NH3)4(NO3)2 and activated by calcination, high temperature hydrogen, or nitrogen treatments. The chemico-physical and structural properties were evaluated by XRD, 1H MAS NMR, ESR, XPS, TG-MS and TEM. The highest H2 evolution rate was observed over P25 based samples and the H2 treatment resulted in more active samples than the other co-catalyst formation methods. In all calcined samples, reduction of Pt occurred during the photocatalytic reaction. Platinum was more easily reducible in all of the P25 supported samples compared to those obtained from the more water-retentive homemade TiO2. This result was related to the negative effect of the adsorbed water content of the homemade TiO2 on Pt reduction and on particle growth during co-catalyst formation.
This study aims to describe the thermal decomposition of two solvatomorphs of decakis(dimethylammonium) dihydrogendodecatungstate ((Me2NH2)10H2W12O42·10H2O and 11 H2O) under inert and oxidizing atmospheres. Thermal studies have been done by TG-MS, TG-DSC-MS, XRD and IR methods in both synthetic air and helium atmospheres. The general characteristics of thermal decomposition are similar for both solvatomorphs. Minor differences could be observed in the resolution and shifting of the decomposition peak temperatures depending on the heating rate or atmosphere used. The first step of decomposition is endothermic in both atmospheres and involves 2 and 5 water molecule elimination with ~ 150 and ~ 120 °C peak temperatures for the decahydrate and undecahydrate, respectively. The elimination of further water and dimethylamine was observed with increasing the temperature, as well as the disruption of the lattice of compounds. Until 300 °C, these processes are endothermic in both atmospheres, and the further decomposition processes at higher temperatures are left endothermic in helium, but become exothermic in synthetic air atmosphere. In helium atmosphere, above 350 °C, a solid-phase quasi-intramolecular redox reaction takes place when the dimethylamine degradation products react with the W=O bonds with formation of oxidative coupling products of the organic fragments and reduced tungsten oxide with WO~2.93 composition. In synthetic air, above 350 °C, burning of organic fragments takes place, there are no oxidative coupling products and reduced tungsten oxide formation, and the end product of decomposition is monoclinic WO3.
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