Search results for "Supercritical fluid"
showing 10 items of 166 documents
Hydrothermal growth of ZnO nanostructures in supercritical domain: Effect of the metal salt concentration (Zn(NO3)2) in alkali medium (KOH)
2015
Abstract The metal salt concentration effect on the size and morphology of ZnO NPs was highlighted through its synthesis thanks to a continuous one-step method at 401 ± 15 °C and 306 ± 8 bar. Experiments were performed from Zn(NO3)2 and KOH as reactants in concentration ranges of 10–480 mM and 40–1920 mM, respectively. A constant [KOH]/[Zn(NO3)2] ratio of 4 was fixed in order to maintain a constant pH value between 12.5 and 13.0. The as-prepared NPs were characterized by X-ray diffraction and (high-resolution) transmission electron microscopy. Based on Louer's method, ZnO crystal exhibiting a hexagonal structure was considered as cylinder with a diameter D and a height H. The D/H parameter …
Continuous hydrothermal synthesis of nanometric BaZrO3 in supercritical water
2007
Abstract Nanocrystalline barium zirconate (BaZrO 3 ) was synthesized using a hydrothermal synthesis process working in supercritical conditions and in a continuous way. By this method, we succeeded in the continuous and rapid production of nanopowders. As a preliminary work three barium precursors have been investigated: barium hydroxide (Ba(OH) 2 ), barium acetate (Ba(CH 3 COO) 2 ) and barium nitrate (Ba(NO 3 ) 2 ). Two of them (Ba(CH 3 COO) 2 and Ba(NO 3 ) 2 ) led to the pure perovskite phase. Then an experimental design has been conducted in order to determine the influence of the experimental parameters on the crystallinity and the grain size of the final product.
Characteristics of LiFePO4 obtained through a one step continuous hydrothermal synthesis process working in supercritical water
2009
International audience; The olivine-like material LiFePO4 was prepared via a continuous hydrothermal synthesis process working from subcritical to supercritical water conditions. The influence of some processing parameters–temperature and reaction time–was investigated in terms of material purity, grain size and morphology. Supercritical conditions were found to be attractive to synthesize in one step a well-crystallized material without impurities. The primary particles size was in the nanometric range. They showed a natural tendency to form micron size agglomerates, which were supposed to be the cause of the limited capacity, as demonstrated through a cross study using laser particle size…
The rate of polymerization in two loci reaction systems: VDF-HFP precipitation copolymerization in supercritical carbon dioxide
2011
When the copolymerization of vinylidene fluoride (VDF) and hexafluoropropylene (HFP) is carried out in supercritical carbon dioxide (scCO 2) under heterogeneous conditions, the reaction occurs both in the continuous CO 2-rich phase and in the dispersed polymer-rich phase. The two phases being characterized by different values of reactant concentrations and kinetic parameters, one would expect that the reaction kinetics is affected by the polymer phase holdup in the reactor. However, the reaction rate is almost insensitive to the amount of produced polymer, at least at specific reaction conditions. This apparent contradiction is discussed and clarified in this paper by a series of comparativ…
A one-pot method to enhance dissolution rate of low solubility drug molecules using dispersion polymerization in supercritical carbon dioxide
2009
The surfactant assisted polymerization of 1-vinyl-2-pyrrolidone in supercritical carbon dioxide in the presence of Piroxicam, selected as a model of a low aqueous solubility drug, was studied in order to prepare in a single step a polymeric composite to enhance the rate of dissolution of the pharmaceutical compound. Reactive entrapping was carried out at 65 degrees C in the P range 21-38MPa. Under proper operative conditions we obtained the composite under the form of sub-micron spherical particles with relatively narrow particle size distribution. Drug loadings higher than 12% (w/w) were obtained and XRD and Raman spectroscopy suggest that the anti-inflammatory agent is dispersed in the ma…
Fixed Bed Adsorption of Drugs on Silica Aerogel from Supercritical Carbon Dioxide Solutions
2013
Supercritical adsorption coupled with the high adsorption capacity of silica aerogel allows the preparation of a new kind of delivery systems of poor water soluble drugs. In order to overcome drawbacks of conventional techniques where the use of liquid solvents can cause the fracture of aerogel porous structure, in this work a new adsorption process of drugs from a supercritical mixture is proposed. Adsorption takes place from a fluid solution of the drug in supercritical CO2and ethanol as cosolvent. A fixed bed adsorption plant has been developed to allow fast mixing of fluid phase and effective contact in the adsorption column. The use of ethanol as cosolvent allows to overcome the limita…
Spherical microparticles production by supercritical antisolvent precipitation: Interpretation of results
2008
Abstract Supercritical antisolvent micronization has been the subject of many works aimed at the production of precipitates with controlled particle size and morphology. Several morphologies have been observed; but, the production of spherical micrometric particles has been the major objective of most of the studies performed. Therefore, in this work, literature data analysis on spherical and related morphologies has been performed. The ranges of process conditions at which spherical microparticles have been obtained have been listed and discussed. A possible formation mechanism is proposed that is based on the competition between jet break-up and liquid surface tension vanishing characteri…
Solubility of the assemblage albite+K-feldspar+andalusite+quartz in supercritical aqueous chloride solutions at 650 °C and 2 kbar
2003
Abstract The solubility of the high grade pelite assemblage albite+K-feldspar+andalusite+quartz at 650 °C and 2 kbar was determined in aqueous solutions over a total chloride range of 0.01–3 mCltot using rapid-quench hydrothermal technique. The concentration of Na, K, Si, and Al was determined in the fluid phase after quench. The K/Na ratio was determined by approaching the equilibrium from below and above. It is 0.34 at low chloride concentrations and decreases slightly to 0.31 with increasing total chloride. Silica and aluminum concentrations were determined only from undersaturation. The silica solubility is found to be independent of chloride concentration and is ∼0.13 molal. Aluminum i…
Silver-Catalyzed C-C Bond Formation between Methane and Ethyl Diazoacetate in Supercritical CO2
2011
Even in the context of hydrocarbons’ general resistance to selective functionalization, methane’s volatility and strong bonds pose a particular challenge. We report here that silver complexes bearing perfluorinated indazolylborate ligands catalyze the reaction of methane (CH4) with ethyl diazoacetate (N2CHCO2Et) to yield ethyl propionate (CH3CH2CO2Et). The use of supercritical carbon dioxide (scCO2) as the solvent is key to the reaction’s success. Although the catalyst is only sparingly soluble in CH4/CO2 mixtures, optimized conditions presently result in a 19% yield of ethyl propionate (based on starting quantity of the diazoester) at 40°C over 14 hours.
Homogeneous Metal-Based Catalysis in Supercritical Carbon Dioxide as Reaction Medium
2016
Above 31.1 degrees C and 73.8 bar, carbon dioxide reaches the supercritical state, being transformed into a fluid (scCO(2)) that has attracted interest in the last few decades as reaction medium for several transition-metal-catalyzed organic transformations. The main feature of this fluid rests on its capability to dissolve large amounts of other gases such as hydrogen, carbon monoxide, ethylene, or even methane and light alkanes. In this manner, very high concentrations of these reactants are available for catalysis. In this contribution a review of the main achievements of the use of transition-metal complexes as catalysts in scCO(2) is presented.