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1.
Chemosphere ; 339: 139583, 2023 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-37480955

RESUMO

A solvothermal method was used to synthesize the mesoporous TiO2, (1-3w %) Cu-doped mesoporous TiO2 membrane with the help of a bioreactor. To understand the physicochemical composition of all synthesized nanomaterials, the structure, morphology and crystallinity of the materials were studied using X-ray diffractometer (XRD), Field emission scanning electron microscopy (FESEM), Fourier transform-infrared (FTIR), Energy dispersive X-ray spectroscopy (EDS) and cyclic voltammetry (CV). Under artificial light source (500 W mercury bulb) irradiations, the nano catalysts' catalytic effectiveness was examined for the azo dyes, namely Congo red. Cu-doping causes a shift in the light absorption of mTiO2 from the ultraviolet to the visible region. The 3w% Cu-doped mTiO2 photocatalyst exhibits lower band gap energy (2.6eV) than TiO2 which is 3.2 eV to efficiently utilize solar energy. As a result, the light absorption was shifted towards the visible spectrum. The recommended mTiO2 and (1, 2, 3) w% Cu-doped mTiO2 photocatalysts were used to photodegrade Congo red and methylene blue. For the degradation of CR, the mTiO2 photocatalyst exhibited 61% and 3w% Cu-doped mTiO2 demonstrated 99% photocatalytic performance after 50 min. A variety of scavengers were also utilized to distinguish the active species by catching the radicals and holes created during the process of photocatalytic degradation. CV indicates the presence of Cu2+ and Cu1+ in Cu-doped mTiO2. Oxygen vacancies and the electronegative surface of Cu1+ seem to perform the photocatalytic reduction of CR.


Assuntos
Vermelho Congo , Luz , Titânio/química , Corantes , Catálise
2.
Molecules ; 28(8)2023 Apr 08.
Artigo em Inglês | MEDLINE | ID: mdl-37110553

RESUMO

Lithium-ion batteries (LIBs) have been explored to meet the current energy demands; however, the development of satisfactory anode materials is a bottleneck for the enhancement of the electrochemical performance of LIBs. Molybdenum trioxide (MoO3) is a promising anode material for lithium-ion batteries due to its high theoretical capacity of 1117 mAhg-1 along with low toxicity and cost; however, it suffers from low conductivity and volume expansion, which limits its implementation as the anode. These problems can be overcome by adopting several strategies such as carbon nanomaterial incorporation and polyaniline (PANI) coating. Co-precipitation method was used to synthesize α-MoO3, and multi-walled CNTs (MWCNTs) were introduced into the active material. Moreover, these materials were uniformly coated with PANI using in situ chemical polymerization. The electrochemical performance was evaluated by galvanostatic charge/discharge, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). XRD analysis revealed the presence of orthorhombic crystal phase in all the synthesized samples. MWCNTs enhanced the conductivity of the active material, reduced volume changes and increased contact area. MoO3-(CNT)12% exhibited high discharge capacities of 1382 mAhg-1 and 961 mAhg-1 at current densities of 50 mAg-1 and 100 mAg-1, respectively. Moreover, PANI coating enhanced cyclic stability, prevented side reactions and increased electronic/ionic transport. The good capacities due to MWCNTS and the good cyclic stability due to PANI make these materials appropriate for application as the anode in LIBs.

3.
Chemosphere ; 315: 137659, 2023 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-36603674

RESUMO

Direct hydrazine liquid fuel cell (DHFC) is perceived as effectual energy generating mean owing to high conversion efficiency and energy density. However, the development of well-designed, cost effective and high performance electrocatalysts is the paramount to establish DHFCs as efficient energy generating technology. Herein, gamma alumina supported copper oxide nanocatalysts (CuO/Al2O3) are synthesized via impregnation method and investigated for their electrocatalytic potential towards hydrazine oxidation reaction. CuO with different weight percentages i.e., 4%, 8%, 12%, 16% and 20% are impregnated on gamma alumina support. X-ray diffraction analysis revealed the cubic crystal structure and nanosized particles of the prepared metal oxides. Transmission electron microscopy also referred to the cubic morphology and nanoparticle formation. Electrochemical oxidation potential of the CuO/Al2O3 nanoparticles is explored via cyclic voltammetry as the analytical tool. Optimization of conditions and electrocatalytic studies shown that 16% CuO/Al2O3 presented the best electronic properties towards N2H2 oxidation reaction. BET analysis ascertained the high surface area (131.2546 m2 g1) and large pore diameter (0.279605 cm³ g-1) for 16% CuO/Al2O3. Nanoparticle formation, high porosity and enlarged surface area of the proposed catalysts resulted in significant oxidation current output (600 µA), high current density (8.2 mA cm-2) and low charge transfer resistance (3.7 kΩ). Electrooxidation of hydrazine on such an affordable and novel electrocatalyst opens a gateway to further explore the metal oxide impregnated alumina materials for different electrochemical applications.


Assuntos
Cobre , Nanopartículas , Cobre/química , Óxido de Alumínio/química , Nanopartículas/química , Óxidos , Hidrazinas
4.
ACS Omega ; 7(27): 23643-23652, 2022 Jul 12.
Artigo em Inglês | MEDLINE | ID: mdl-35847279

RESUMO

Simvastatin (SIM) is a diet drug to treat high lipid levels in the blood. It has the drawback of being metabolized in humans' gastrointestinal tract (GIT) when taken in an oral dosage form. To enhance the role of SIM in treating hyperlipidemias and bypassing its metabolism in GIT, a biodegradable nanocarrier as a SIM-loaded lipid emulsion nanoparticle via the solvent injection method was designed. Cholesterol acts as a lipid core, and Tween 80 was utilized to stabilize the core. The optimized nanoformulation was characterized for its particle diameter, zeta potential, surface morphology, entrapment efficiency, crystallinity, and molecular interaction. Furthermore, the transdermal hydrogel was characterized by physical appearance, rheology, pH, and spreadability. In vitro assays were executed to gauge the potential of LENPs and olive oil for transdermal delivery. The mean particle size and zeta potential of the optimized nanoparticles were 174 nm and -22.5 mV 0.127, respectively. Crystallinity studies and Fourier transform infrared analyses revealed no molecular interactions. Hydrogels showed a sustained release compared to SIM-loaded LENPs that can be proposed as a better delivery system for SIM. We encourage further investigations to explore the effect of reported formulations for transdermal delivery by in vivo experiments.

5.
Artigo em Inglês | MEDLINE | ID: mdl-33442283

RESUMO

To look superior and acceptable in society, people from all over the world use various types of cosmetic products to enhance or alter their facial appearance and body texture. In recent times, an exponential surge in cosmetic use has been observed in Pakistan, and hence spending money on personal-care products is high. However, there are many reported facts about high loads of lead, mercury, copper, and others hazardous and cancerous elements in local Pakistani cosmetic brands. Consumers of these brands are at high risk of many clinical issues, including cancer. As such, it is a necessity to make people aware of the devastating harmful effects related to cosmetic use. The aim of this study was to provide information for stakeholders and raise awareness in the general public about the use of these local unauthorized personal-care cosmetic products, along with government strategies to stop this cosmetic blight on human health.

6.
Recent Pat Nanotechnol ; 10(3): 221-230, 2016.
Artigo em Inglês | MEDLINE | ID: mdl-27136932

RESUMO

BACKGROUND: Sulfonated polyimides (SPIs) are considered as the promising alternatives to Nafion as membrane materials for the polymer electrolyte membrane (PEM). They generally exhibit high ionic conductivity, good mechanical properties, excellent thermal and chemical stabilities. The six-membered ring, naphthalenic anhydride-based SPIs, not only exhibit superior chemical and thermo-oxidative stabilities but are also more resistant to hydrolysis than their five-membered phthalic anhydride-based SPIs. The composites based on napthalenic polyimides are also significantly stable in high temperature environment and show better stability to hydrolysis. Incorporation of inorganic fillers into organic polymers has gained tremendous attention and these new materials are called organic-inorganic hybrids. Few patents related to the synthesis and performance PEM materials have been reviewed and cited. Keeping in view the importance of sulfonated polyimide based nanocomposites as potential membrane materials for PEM in fuel cell, we have synthesized SPIs clay based nanocomposite as potential membrane material. The objective of this work was to synthesize clay based SPIs thin films which could be used as membrane materials in PEM fuel cell for energy applications. Methods/Experimental: At the first step the nanometric sheets of vermiculite clay prepared via sonication was surface modified by grafting 3-APTES. Then the SPI was synthesized via one-step high temperature direct imidization method, which serve as a matrix material. The organo modified VMT was dispersed via sonication in the SPI matrix. Four different sets of organic-inorganic nanocomposite membranes thin films, having VMT contents in the range of 1 to 7 wt.% were prepared by casting, curing and acidification route. RESULTS: The synthesis of SPIs clay based thin films were carried out at three different steps and fully characterized. The synthesis of SPIs and SPIs clay based thin films were analyzed via different analytical techniques. The XRD analysis tells the successful dispersion of clay in SPI matrix. Different physiochemical tests were conducted for the analysis of these membranes such as water uptake, hydrolytic stability, ion exchange capacity (IEC), dimensional changes and oxidative stability, to check their suitability as membrane materials for PEM. The proton conductivity of these membranes were measured via impedance spectroscopy which discloses three different active regions responsible for proton conduction. The activation energies of the membranes were higher at lower temperature and reaches to 8.2 kJ/mol at higher temperature (90oC). CONCLUSION: The synthesis of sulfonated polyimide/clay (SPI/clay) based organic-inorganic nanocomposite membranes were achieved successfully. The membrane display good hydrolytic, thermal and oxidative stability at elevated temperature. The proton conductivity of the membrane display an increase together with the frequency but decreases with temperature. Therefore some more efforts are required to achieve high degree of functionalization of both organic and inorganic components, for the "future" PEMs to avoid deterioration and to get improved performance.

7.
Ultrason Sonochem ; 21(3): 1002-9, 2014 May.
Artigo em Inglês | MEDLINE | ID: mdl-24262759

RESUMO

The effects of temperature, time, solvent and sonication conditions under air and Argon are described for the preparation of micron and sub-micron sized vermiculite particles in a double-jacketed Rosett-type or cylindrical reactor. The resulting materials were characterized via X-ray powder diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM), Fourier Transform Infrared (FTIR) Spectroscopy, BET surface area analysis, chemical analysis (elemental analysis), Thermogravimetry analysis (TGA) and Laser Granulometry. The sonicated vermiculites displayed modified particle morphologies and reduced sizes (observed by scanning electron microscopy and laser granulometry). Under the conditions used in this work, sub-micron sized particles were obtained after 5h of sonication, whereas longer times promoted aggregation again. Laser granulometry data revealed also that the smallest particles were obtained at high temperature while it is generally accepted that the mechanical effects of ultrasound are optimum at low temperatures according to physical/chemical properties of the used solvent. X-ray diffraction results indicated a reduction of the crystallite size along the basal direction [001]; but structural changes were not observed. Sonication at different conditions also led to surface modifications of the vermiculite particles brought out by BET surface measurements and Infrared Spectroscopy. The results indicated clearly that the efficiency of ultrasound irradiation was significantly affected by different parameters such as temperature, solvent, type of gas and reactor type.

8.
J Colloid Interface Sci ; 363(2): 490-6, 2011 Nov 15.
Artigo em Inglês | MEDLINE | ID: mdl-21868022

RESUMO

A viable cost-effective approach employing mixtures of non-ionic surfactants Triton X-114/Triton X-100 (TX-114/TX-100), and subsequent cloud point extraction (CPE), has been utilized to concentrate and recycle inorganic nanoparticles (NPs) in aqueous media. Gold Au- and palladium Pd-NPs have been pre-synthesized in aqueous phases and stabilized by sodium 2-mercaptoethanesulfonate (MES) ligands, then dispersed in aqueous non-ionic surfactant mixtures. Heating the NP-micellar systems induced cloud point phase separations, resulting in concentration of the NPs in lower phases after the transition. For the Au-NPs UV/vis absorption has been used to quantify the recovery and recycle efficiency after five repeated CPE cycles. Transmission electron microscopy (TEM) was used to investigate NP size, shape, and stability. The results showed that NPs are preserved after the recovery processes, but highlight a potential limitation, in that further particle growth can occur in the condensed phases.


Assuntos
Ouro/química , Nanopartículas Metálicas/química , Octoxinol/química , Paládio/química , Polietilenoglicóis/química , Tensoativos/química , Fracionamento Químico , Reutilização de Equipamento , Ligantes , Mesna/química , Tamanho da Partícula , Reciclagem , Propriedades de Superfície
9.
J Colloid Interface Sci ; 354(2): 624-9, 2011 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-21134683

RESUMO

Water-in-oil microemulsions (w/o µEs) stabilized by the cationic surfactant cetyltrimethylammonium chloride (CTACl) have been used as reaction media to generate Au nanoparticles (Au-NPs). In addition the pure µEs have been used as media to disperse Au and Pd-NPs, which have been pre-synthesised in aqueous phases and stabilized by sodium 2-mercaptoethanesulfonate (MES) ligands, and also commercially available SiO(2)-NPs. A general method for recovery and separation of the nanoparticles from these mixed NP-µE systems has been demonstrated by tuning phase behavior of the background microemulsions. Addition of appropriate aliquots of water drives a clean liquid-liquid phase transition, resulting in two macroscopic layers, the NPs preferentially partition into an upper oil-rich phase and are separated from excess surfactant which resides in a lower aqueous portion. UV-vis and (1)H NMR spectroscopy have been used to follow these separation processes and quantify the recovery and recycle efficiencies for the different NPs. For example, ∼90% of the microemulsion-prepared Au-NPs can be recovered; with even greater separation efficiencies attainable for pre-synthesised MES-stabilized Au-MES-NPs (∼98%) and Pd-MES-NPs (92%). For the silica NP-µE dispersions gravimetry indicates ∼84% recovery of the NPs. TEM images of all systems showed that NP shapes and size distributions were generally preserved after these phase transfer processes. This low-energy and cost-effective purification route appears to be a quite general approach for processing different inorganic NPs, having advantages of being isothermal, using only commercially available inexpensive components and requiring no additional organic solvents.


Assuntos
Compostos de Cetrimônio/química , Fracionamento Químico/métodos , Ouro/química , Mesna/química , Nanopartículas Metálicas/química , Tensoativos/química , Cetrimônio , Emulsões/química , Nanopartículas Metálicas/ultraestrutura , Paládio/química , Dióxido de Silício/química , Água/química
10.
J Fluoresc ; 20(5): 1049-59, 2010 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-20446023

RESUMO

An approach is demonstrated toward the synthesis of four novel cyclohexenone derivatives (CDs) via a convenient route of Michael addition of ethyl acetoacetate. The molecular structures of CDs were confirmed by means of FT-IR, (1)H NMR, EIMS, UV and also by X-ray single crystal structure analysis. CDs are strongly fluorescent compounds and their fluorescent spectra exhibits intense violet fluorescence. To model the binding to biological membranes the behavior of CDs in micellar solutions of a cationic surfactant, cetyltrimethylammonium bromide (CTAB) and an anionic surfactant, sodium dodecylsulfate (SDS) has also been examined. The characteristics of partition and binding interactions of CDs with CTAB and SDS were investigated by UV-Visible and fluorescence spectroscopic techniques. Higher values of all mentioned interactions in case of CTAB, compared to SDS, indicate that there are greater interactions between the CDs and CTAB than with SDS.


Assuntos
Corantes/síntese química , Íons , Micelas , Cetrimônio , Compostos de Cetrimônio/química , Corantes/química , Espectroscopia de Ressonância Magnética/métodos , Dodecilsulfato de Sódio/química , Espectrometria de Massas por Ionização por Electrospray/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos , Tensoativos/química , Raios X
11.
AAPS PharmSciTech ; 10(4): 1286-94, 2009.
Artigo em Inglês | MEDLINE | ID: mdl-19876741

RESUMO

Formulation of a new oil-in-water (o/w) microemulsion composed of castor oil/Tween 80/ethanol/phosphate buffer for enhancing the loading capacity of an anti-inflammatory drug piroxicam has been accomplished. The pseudo-ternary phase diagram has been delineated at constant surfactant/cosurfactant ratio (1:2). The internal structure of so created four-component system was elucidated by means of an analysis of isotropic area magnitudes in the phase diagram. Conductivity (sigma), kinematic viscosity (keta), and surface tension (gamma) studies with the variation in Phiw (weight fraction of aqueous phase) show the occurrence of structural changes from water-in-oil (w/o) microemulsion to oil-in-water (o/w). Along with the solubility and partition studies of piroxicam in microemulsion components, the changes in the microstructure of the microemulsion after incorporation of drug have been evaluated using pH, sigma, gamma, keta, and density studies. Piroxicam, a poorly water-soluble drug displayed high solubility (1.0%) in an optimum microemulsion formulation using ethanol (55.0%), Tween 80 (26.5%), castor oil (7.5%), and phosphate buffer (11.0%). The results have shown that the microemulsion remained stable after the incorporation of piroxicam. Fluorescence spectra analysis taking pyrene as fluorescent probe was performed, and the results showed that pyrene was completely solubilized in the oil phases of the bicontinuous microemulsions. The fluorescence spectrum of the model drug piroxicam was used to probe the intramicellar region of nonionic microemulsion. The results showed that the piroxicam was localized in the interfacial film of microemulsion systems more deeply in the palisade layer with ethanol as the cosurfactant.


Assuntos
Anti-Inflamatórios não Esteroides/química , Piroxicam/química , Condutividade Elétrica , Emulsões , Fluorescência , Micelas , Piroxicam/administração & dosagem , Solubilidade , Tensão Superficial , Viscosidade
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