Facile synthesis and thermal properties of waterglass-based silica xerogel nanocomposites containing reduced graphene oxide

In this study, new rGO-silica xerogel nanocomposites (SX-rGO) and its glass fiber reinforced composites (GFR-SX-rGO) were prepared, and its microstructure and thermal properties were evaluated. The raw material was a mixed dispersion prepared by adding 0.01–2.5?wt% of reduced graphene oxide (rGO) to waterglass (6% SiO₂). A hydrogel was prepared via sol-gel reaction of this raw material, which was then immersed in hydrochloric acid, hydrophobized in a siloxane/2-propanol reaction system, and then dried at ambient pressure to obtain a hydrophobic carbon-silica xerogel composite. The obtained samples were characterized by N₂ physisorption (at 77?K), solid ²⁹Si Magic angle spinning nuclear magnetic resonance spectroscopy, Fourier-transform infrared spectroscopy, Raman spectroscopy, differential scanning calorimetry, thermogravimetric analysis, hydrophobicity, and thermal conductivity. It was found that as the amount of rGO was increased, the specific surface area of the nanocomposite decreased by ~25% from 535 to 403?cm²/g, and the average pore size and pore volume were almost halved. The thermal decomposition temperature of the SX-rGO was increased markedly by the addition of rGO. Moreover, the GFR-SX-rGO-0.5 showed low density (0.208?g/cm³), high contact angle (146°) and low thermal conductivity (0.0199?W/mK).     

Natural polysaccharides platforms for oral controlled release of ketoprofen lysine salt

Context: Ketoprofen lysinate (KL) is one of the most widely used non-steroidal anti-inflammatory drugs in the symptomatic treatment of some chronic inflammatory diseases. Compared to ketoprofen, KL shows better pharmacokinetics and tolerability. However, due to its short half-life of 1–2?h, a multiple dose regimen is required for oral administration. Thus, the present work deals with its encapsulation in a hydrogel-based system by prilling in order to prolong its activity.

Objective: In this paper, we propose alginate and pectin as carriers and release tailoring agent for the development of hydrogel-based beads for KL retarded and sustained release.

Materials and methods: Beads were produced by a Nisco Encapsulator® using alginate or pectin. Operative variables were optimized to produce beads with desired morphology and size. Solid state properties were analyzed by SEM and DSC. Drug release performance was studied by Pharmacopeia pH-change assay to simulate gastrointestinal environment.

Results and discussion: Prilling technique was successfully used to encapsulate high soluble drugs as KL in polysaccharides-based hydrogels. Pectin proved to be a proper polymer able to encapsulate ketoprofen lysine salt. Formulation (F8) showed good morphological properties and size, high drug content (15.6%) and encapsulation efficiency (93.5%) and promising drug release profiles. Hosting F8 in an acid-resistant capsule (DR^®caps) a delivery platform has been developed to control KL release in a delayed (90?min lag time) and prolonged way (270?min complete release).

Conclusion: The platform may be proposed as potentially useful in the oral administration of NSAIDs in chronic inflammatory diseases affected by circadian rhythm.     

Influence of support’s oxygen functionalization on the activity of Pt/carbon xerogels catalysts for methanol electro-oxidation

Highly mesoporous carbon xerogels (CXs) were synthesized using two different resorcinol to catalyst, R/C, molar ratios and functionalized with different oxidation treatments. The synthesized carbon materials were used as supports for Pt particles, deposited by impregnation and reduction in formic acid. Both carbon supports and the catalysts prepared were characterized by means of N₂ physisorption, scanning and transmission electron microscopy, temperature programmed desorption and X-ray diffraction. The electrochemical activity of the catalysts towards the oxidation of carbon monoxide and methanol was assayed by means of cyclic voltammetry and chronoamperometry. Textural characterization of the materials prepared evidenced more developed and mesopore-enriched porous structure for the carbon xerogel prepared using the highest R/C molar ratio. Enhanced textural properties of this material led to the preparation of highly active Pt-catalysts, which showed increased tolerance to CO and higher activity in methanol electro-oxidation, in comparison to Pt-E-TEK and the catalysts prepared in an analogous way using Vulcan XC-72R carbon black as support. Functionalization treatments resulted in enhanced dispersion, lower Pt crystal size and improved catalytic performance in the case of the catalysts prepared using the carbon xerogel possessing a less developed porous structure. Pt agglomeration was found to strongly determine the activity of the catalysts prepared. At high potentials, i.e. 1 V vs. RHE, the catalyst prepared using the carbon xerogel submitted to the most stringent oxidation treatment showed the highest specific peak activity towards methanol electro-oxidation, probably due to the positive influence of the presence of oxygen surface groups in Pt-carbon interaction, in spite of the higher agglomeration extent confirmed by TEM. On the other hand, at 0.60 V vs. RHE, highest activity towards methanol electro-oxidation was determined for the catalysts prepared using the non-functionalized carbon xerogel which can be explained in terms of enhanced reactant/product diffusion together with intrinsic higher catalytic activity due to lower Pt crystal size. In any case, the activity of this catalyst prepared using a carbon xerogel as support was found to be more than 2 times higher than the one determined for Pt/E-TEK, confirming the considerable improvement of the electrocatalytic system by means of optimization of the carbon support employed.     

Hydrogen production by steam reforming of liquefied natural gas (LNG) over mesoporous nickel–alumina xerogel catalysts prepared by a single-step carbon-templating sol–gel method

A series of mesoporous nickel–alumina xerogel catalysts (denoted as CNAX) were prepared by a single-step carbon-templating sol–gel method using different amount of carbon template (X), and they were applied to the hydrogen production by steam reforming of liquefied natural gas (LNG). Textural properties of CNAX catalysts were improved with increasing the amount of carbon template. CNAX catalysts exhibited diffraction peaks corresponding to nickel aluminate phase, while CNA18 and CNA24 catalysts showed additional bulk nickel oxide phase. From TPR measurements, it was revealed that the interaction between nickel species and alumina in the CNAX catalysts became weakened with increasing the amount of carbon template. Crystallite size of metallic nickel in the reduced CNAX catalysts showed a volcano-shaped trend with respect to the amount of carbon template. In the steam reforming of LNG, CNAX (X = 0, 6, 12, and 18) catalysts exhibited a stable catalytic performance during the reaction, while CNA24 catalyst showed a significant catalyst deactivation. Crystallite size of metallic nickel served as an important factor determining the catalytic performance in the steam reforming of LNG. Initial LNG conversion and initial hydrogen yield increased with decreasing crystallite size of metallic nickel of the catalysts. Among the catalysts tested, CNA12 catalyst with the smallest crystallite size of metallic nickel showed the best catalytic performance.     

Preparation of silica xerogel with high silanol content from sodium silicate and its application as CO2 adsorbent

In this study, silica xerogels with high silanol content were synthesized by using sodium silicate as low-cost silica source in the presence of hydrochloric acid and acetic acid via sol–gel process for CO₂ adsorption purpose. The effect of amount of acetic acid on the surface and structural properties of silica xerogel was investigated. Fourier transform infrared spectroscopy (FTIR) and thermal gravimetric analysis (TGA) revealed that the silanol groups existed on the surface of silica xerogel products and their concentration increased with increasing the amount of acetic acid. The BET surface area and total pore volume of the silica xerogel prepared using 6 mL of acetic acid (MMS-6) were found to be 1021 m²/g and 0.72 cm³/g, respectively. The pore structure of silica xerogel products consisted of the interparticle voids between the nanoparticles aggregates, and the interconnected wormhole microporous structure. The latter pore structure was more uniform on increasing the amount of acetic acid. CO₂ adsorption/desorption measurements were carried out using TGA unit with high purity CO₂ (99.999%). The highest CO₂ sorption capacity (83.6 mg_CO2/g_sorbent) was obtained with MMS-6 product. Thermal swing adsorption studies showed that the silica xerogel products exhibited strongly reversible CO₂ adsorption capacity and stable during 5-repeated cycle of adsorption/desorption experiment at 35 °C.     

Transport Properties of K_xV_2O_5·nH_2O Nanocrystalline Films

Five different compositions of K x V 2 O 5 ·nH 2 O(where x=0.00,0.0017,0.0049,0.0064 and 0.0091 mol) were prepared by the sol-gel process.Electrical conductivity and thermoelectric power were measured parallel to the substrate surface in the temperature range of 300-480 K.The electrical conductivity showed that all samples were semiconductors and that conductivity increased with increasing K content.The conductivity of the present system was primarily determined by hopping carrier mobility.The carrier density was evaluated as well.The conduction was confirmed to obey non-adiabatic small polaron hopping.The thermoelectric power or Seebeck effect,increased with increasing K ions content.The results obtained indicated that an n-type semiconducting behavior within the temperature range was investigated.     

Stable support based on highly graphitic carbon xerogel for proton exchange membrane fuel cells

Highly graphitic carbon xerogel (GCX) is prepared by the modified sol-gel polymerization process using cobalt nitrate as the catalyst, followed by high temperature treatment at 1800 °C. The as-prepared GCX is explored as a stable support for Pt in proton exchange membrane fuel cells. The results of N₂ sorption measurement and X-ray diffraction analysis (XRD) reveal that GCX has a better mesoporous structure and a preferably higher degree of graphitization, compared with the commercial XC-72 carbon black. The transmission electron microscopy (TEM) image indicates that Pt nanoparticles are well dispersed on GCX and exhibit relatively narrow size distribution. Accelerated aging test (AAT) based on potential cycling is used to investigate the durability of the as-prepared Pt/GCX in comparison with the commercial Pt/C. Electrochemical analysis demonstrates that the catalyst with GCX as a support exhibits an alleviated degradation rate of electrochemical active surface area (39% for Pt/GCX and 53% for Pt/C). The results of single cell durability tests indicate that the voltage loss of Pt/GCX at 100 mA cm⁻² is about 50% lower than that of Pt/C. GCX is expected to be a corrosion resistant electrocatalyst support.     

Hydrothermal synthesis of hydrated vanadium oxide nanobelts using poly (ethylene oxide) as a template

With the aim of obtaining nanodevices as batteries, sensors and fuel cells, we prepared V₂O₅ and V₃O₇·H₂O nanobelts by a simple hydrothermal process using poly (ethylene oxide) (PEO) as a template. The yielding percentage of the nanomaterial is less in polymer-free V₂O₅ nanobelts and material size is also big. It is apparent that PEO used V₃O₇·H₂O form a continuous and relatively homogeneous matrix with a clearly 1–5 μm long and 50–150 nm diameter nanobelts morphology. The SEM micrographs suggest that there is no bulk deposition of polymer on the surface of the nano-crystallites. Strong interaction between the vanadyl group and the polymer during the formation process has been identified by the shifts of the vanadyl vibration peaks. The CV curve of the electrode made of the V₃O₇·H₂O nanobelts have higher current densities than the CV curve of the electrode made of V₂O₅ nanobelts.