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Treatment of dye pollutants prior to their release into the environment remains a formidable challenge, persisting as a longstanding issue. This study focuses on the development of a multiwalled carbon nanotube-foam (MWCNT-foam) composite through low-temperature chemical fusion (LTFC), resulting in a composite with a remarkably high accessible surface area (>475 m2 g-1). The MWCNT-foam composite exhibits a three-dimensional porous structure and demonstrates a notable affinity for organic dye adsorption. The efficacy of this composite was evaluated against various cationic dyes such as Methylene blue (MB) and Crystal Violet (CV) as well as anionic dyes such as Congo red (CR) and Eriochrome black T (EB), and the composite showed removal rates exceeding 99%. Furthermore, the study delved into the impact of the initial dye concentration, adsorbent dosage, kinetics, and other factors on the performance of the MWCNT-foam composite. The adsorption process achieved equilibrium in 10 min and strongly correlated with the pseudo-second-order kinetic model and Langmuir isotherm. The maximum adsorption capacity of MWCNT-foam for MB, CV, CR, and EB was found to be 168.63, 147.49, 99.50, and 93.11 mg g-1, respectively. In order to showcase the potential of this material for continuous adsorption, a specialized cartridge was designed and employed to treat dye solutions, demonstrating the feasibility of continuous mode adsorption.
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The present work studied the decomposition of isopropyl alcohol (IPA), widely used in chemical industries and households, in a packed-bed dielectric barrier discharge (DBD) plasma reactor. Metal oxide (MOx) coated on γ-Al2O3 (M = Cu, Mn, Co) was utilized for packing. The plasma-packed mode was a likely alternative to the conventional removal techniques, as it aids the conversion of dilute concentrations of IPA to CO and CO2 at ambient conditions (room temperature and atmospheric pressure). The mean electron energy calculations suggest that electrons with higher energy are generated when the discharge zone is packed with catalysts. When comparing IPA conversion (input concentration of 25 ppm) for no packing mode and MOx/γ-Al2O3 coupled plasma mode, the latter method enhances conversion to greater than 90% at an applied voltage of 18 kV. Also, MOx/γ-Al2O3 showed the highest selectivity to CO2 (70%) compared to plasma-only mode (45%). The metal-oxide layer provides the necessary catalytic surface facilitating the oxidation of IPA to COx through active oxygen species or the interaction of surface hydroxyl groups. The use of MOx/γ-Al2O3 resulted in about 90% carbon balance and reduced ozone generation, demonstrating the significance of integrating metal oxide to achieve efficient conversion and maximal selectivity towards the desired products.
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Eco-friendly carbothermal techniques were used to synthesize nanocomposites of biowaste-derived Ni/NiO decorated-2D biochar. The use of chitosan and NiCl2 in the carbothermal reduction technique was a novelty to synthesize the Ni/NiO decorated-2D biochar composite. Potassium persulfate (PS) was found to be activated by Ni/NiO decorated-2D biochar, which is thought to oxidize organic pollutants through an electron pathway designed by the reactive complexes formed between PS and the Ni/NiO biochar surface. This activation led to the efficient oxidation of methyl orange and organic pollutants. Analyzing Ni/NiO decorated-2D biochar composite before and after the methyl orange adsorption and degradation procedure allowed us to report on the process of its elimination. The Ni/NiO biochar with PS activation showed higher efficiency than Ni/NiO decorated-2D biochar composite as this material was able to degrade over 99% of the methyl orange dye. The effects of initial methyl orange concentration, dosages effect, solution pH, equilibrium studies, kinetics, thermodynamic studies, and reusability were examined and evaluated on Ni/NiO biochar.
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Poluentes Ambientais , Poluentes Químicos da Água , Adsorção , Compostos Azo/química , Carvão Vegetal/química , Poluentes Químicos da Água/análiseRESUMO
The use of electronic devices and wireless networks is increasing rapidly, and electromagnetic (EM) pollution remediation remains a challenge. We employed a unique approach to fabricate two ultrathin (approx. 53 µm) multilayered assemblies to address this. By sequentially stacking thin films of polyvinylidene difluoride (PVDF) and polycarbonate (PC) nanocomposites and interfacially locking them with a mutually miscible polymer (PMMA, polymethyl methacrylate), materials with enhanced structural properties and electromagnetic interference (EMI) shielding performance can be designed. Utilizing reduced graphene oxide (rGO) and molybdenum disulfide (MoS2) as a template, ferrite was grown on the surface to design two different nanohybrid structures (rGO-Fe3O4 and MoS2-Fe3O4). PVDF was composited with either rGO-Fe3O4 or MoS2-Fe3O4, and multiwall carbon nanotubes (CNTs) were dispersed in the PC component. As PC and PVDF are immiscible, their poor interface would result in inferior structural properties, which can be challenging in designing EMI shielding materials due to cyclic thermal fatigue. Hence, PMMA is sandwiched to interfacially stitch the components (PC and PVDF) and improve interfacial adhesion. This was confirmed using SEM/EDS and Raman mapping/imaging. The mechanical stability of the multilayered assemblies was characterized using a dynamic mechanical analyzer (DMA), and the storage modulus was found to be as high as 2767 MPa at 40 °C (@constant frequency and strain amplitude), for the multilayered film with rGO-Fe3O4 in PVDF, PMMA as a sandwich layer and CNTs in PC. A typical assembly of 9 multilayers (â¼480 µm) with rGO-Fe3O4 in PVDF, and CNTs in PC, and interfacially stitched with PMMA gave rise to a high EMI shield effectiveness (SET) of -26.3 dB @ 26.5 GHz. This unique arrangement of a multilayered assembly suppressed EMI primarily by absorption.
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Miniaturization of electronic devices and systems enhances the complexity of inbuilt circuitry, thereby giving rise to electromagnetic interference (EMI). EMI is a serious cause of concern as it affects the performance of a device, transmission channel, or system. In a quest to find an effective solution to this problem, several materials, apart from the conventional metals, such as carbon derivatives, have been extensively explored recently. In addition to carbon derivatives, hybrid structures such as core-shell, conjugated systems, etc. have also been researched. However, semiconducting fillers have received less attention, especially in this application. Hence, this review article will primarily focus on the systematic understanding of the use of semiconductor-based polymer nanocomposites and how the band gap plays a crucial role in deciding the dielectric properties and subsequently the electromagnetic absorption behavior for shielding applications. Our primary aim is to highlight the mechanism of shielding involved in such nanocomposites in addition to discussing the synthesis and properties that lead to effective shielding. Such nanocomposites containing semiconductors can pave the way for alternate materials for EMI shielding applications that are lightweight, flexible, and easy to integrate.
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Biodiesel was synthesized from Schizochitrium limacinum microalgae with different methylating agents namely, methanol, dimethyl carbonate and methyl acetate. The reactions were conducted at 518-643â¯K at 20â¯MPa and methylating agent to algae ratio at 10:1. The reaction time was varied between 10 and 80â¯min. Conversions of >90% was observed within 40â¯min at 543â¯K for methanol system. However, the conversions were considerably lower for other systems and only 50% was observed with dimethyl carbonate after 30â¯min at 643â¯K, and 40% conversion with methyl acetate after 40â¯min at 643â¯K. The rate constants were obtained by pseudo-first order kinetic model. Based on the variation of rate constants with temperature, Arrhenius equation was used to determine the activation energy of all the three reaction systems. The reaction rates were the highest and lowest for the reaction with methanol and methyl acetate, respectively.
Assuntos
Microalgas , Biocombustíveis , Esterificação , Metanol , TemperaturaRESUMO
The goal of this work was to design a device for rapid screening of crosslinked thermoset polymers. This gradient curing platform is capable of yielding a library of polyesters with systematically varying mechanical and physicochemical properties and the resultant cellular response. A library of poly(xylitolsebacate) polyesters was prepared in this device by differential curing to yield a gradient polymer. The resultant polymer exhibits a gradient in the storage modulus (1 to 5â¯MPa), wettability (70°â¯<â¯water contact angleâ¯<â¯110°), degree of crosslinking, degradation rate (3-25% in 7â¯days), drug release and biological response (ability to support stem cell proliferation and differentiation) from one end of the polymer to the other. Primary human mesenchymal stem cells were cultured to assess the cellular response in vitro. Maximal stem cell proliferation and osteogenesis was observed on the highly crosslinked polyester segments that provide high stiffness, are hydrophobic and are slow degrading as compared to the lower cured counterparts. Under in vivo conditions, this material showed differential response across the gradient without displaying significant concerns for inflammation or infection. This gradient curing device is capable of ascertaining suitable curing conditions to obtain appropriate polymers for application specific requirements. This gradient platform was further used to identify optimal processing parameters to prepare three-dimensional tissue scaffolds such as electrospun fiber mats and porous foams. Thus, this versatile combinatorial platform is well suited for rapid screening of thermoset polymers for biomedical applications.
Assuntos
Tecnologia Biomédica/métodos , Técnicas de Química Combinatória , Polímeros/química , Temperatura , Adulto , Animais , Diferenciação Celular , Módulo de Elasticidade , Humanos , Implantes Experimentais , Masculino , Teste de Materiais , Células-Tronco Mesenquimais/citologia , Osteogênese , Poliésteres/química , Porosidade , Ratos Sprague-Dawley , Engenharia Tecidual , Alicerces Teciduais/químicaRESUMO
Visible light responsive semiconductor-based photocatalysis is known to be an efficient method for the disinfection of bacterial cells. Here, we address the issue of aqueous contamination by persistent pollutants such as antibiotics and antibiotic resistant bacteria (ARB) from an innovative angle. Simultaneous degradation of an antibiotic (chloramphenicol) and antibiotic resistant bacteria (chloramphenicol resistant E. coli) is performed to observe the effect of the presence of antibiotic in the reaction system when it is required for survival of the bacteria. A p-n junction-based ZnO/CuI composite is shown to demonstrate drastic enhancement in photocatalytic activity due to the inbuilt potential barrier suppressing charge carrier recombination. Moreover, an additional driving force for the suppression of recombination was provided by using a potential bias. Hydrothermally grown ZnO/CuI electrode films were characterized to assess optical, electrochemical, physicochemical and structural properties of the composite. Electrochemical impedance spectroscopy and diffuse reflectance spectroscopy were performed to obtain insights into the band bending, band edge potential, band gap and transmittance of the semiconductors. X-ray-based spectroscopic methods and zeta potential measurement demonstrated the surface properties and surface charges of the moieties in the reaction system, allowing us to deduce justifiable conclusions. A model based on the interaction of photogenerated radicals with the bacteria was developed and rate expressions were used to obtain the rate constants for the experimental results. Photoelectrocatalysis and photocatalysis followed first order rate kinetics; however, due to the unavailability of direct hole attack in photolysis, the electrolysis and electrocatalysis followed Langmuir-Hinshelwood kinetics. Bacterial disinfection was confirmed by K+ ion leaching and by structural changes in the membrane observed by FTIR of the cells after the reaction. We also addressed the issue of bacterial adhesion on the films restricting the mobility of radicals to interact with the bacteria, affecting the reusability of the catalyst films. The present work opens a wide avenue to discuss and address the improvement of the reusability of nanomaterial films for bacterial applications by controlling bacterial adhesion.
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Unique optical properties render semiconductor Nb2O5 nanoparticles suitable for light harvesting and photocatalytic applications. This study focuses on determining optical properties such as the band gap, conduction band edge, valence band edge and work function of as-prepared solution combustion synthesized Nb2O5 nanoparticles with the help of UV-vis Diffuse Reflectance spectroscopy (DRS) and ultraviolet photoelectron spectroscopy (UPS) techniques. Phase purity and the oxidation states of the elements present in the material were confirmed from X-ray diffraction (XRD) patterns and X-ray photoelectron spectra (XPS), respectively. Doping semiconductors with different metal ions impacts the activity of the material, and therefore efforts were made to understand the effect on the photocatalytic performance of Nb2O5 due to the incorporation of metal dopants viz. Sr, Y, Zr, and Ag. Lattice parameters were obtained from Rietveld refinement of the XRD patterns. Parameters which are closely related to the photoactivity of the catalysts such as the presence of surface defects, oxygen vacancies, surface area, and charge carrier dynamics were determined from photoluminescence (PL) analysis, Brunauer-Emmett-Teller (BET) surface area measurements and time-resolved fluorescence (TRF) analysis respectively. In addition, the dopant concentrations were optimised for enhanced photocatalytic activity. The doped Nb2O5 nanoparticles showed significant activity towards targeted degradation of organic pollutants like 2-chlorophenol (2-CP) and dye contaminants like methylene blue (MB), orange G (OG) and indigo carmine (IC). This strategy yielded a robust response towards inactivation of E. coli and S. aureus as well. Adsorption and photodegradation of MB followed Lagergren's pseudo 1st order reaction model and the Langmuir Hinshelwood model respectively. Bacterial inactivation and OG, IC and 2-CP photodegradation followed 1st order kinetics. The reusability of the catalyst for 5 cycles was demonstrated. Finally, a plausible mechanism is proposed based on radical trapping experiments and combined analysis of the characterization techniques.
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The effect of methylene blue (MB) modified multiwall carbon nanotubes (MWNTs) on the nucleation and morphology of polyvinylidene fluoride (PVDF) in comparison with the effect of MWNTs was systematically assessed by DSC, 13C NMR, FT-IR, TEM, WAXS and SAXS analysis. TEM analysis of ultra-microtomed samples revealed that MB modification enhanced the dispersibility of MWNTs in PVDF. Further, the nanocomposites were subjected to mechanical rolling and the synergistic effect of processing and fillers on the PVDF morphology (before and after rolling) at different length scales was studied. Both FT-IR and WAXS analyses suggested that mechanical rolling transforms α-PVDF to ß-PVDF (ca. 88%). TEM and two-dimensional WAXS analyses revealed that the MWNTs and ß-crystallites are oriented preferentially along the rolling direction and the degree of orientation is not influenced by the fillers suggesting that crystallite orientation is fully controlled by mechanical rolling. On the other hand, ß-lamellae showed perpendicular orientation with respect to the rolling direction. Unlike ß-crystallites, the ß-lamellar morphology and orientation are highly governed by the fillers as evident from SAXS analysis. Using MWNTs and the MWNT-MB π-complex, we demonstrate that the ß-lamellar morphology and degree of orientation are controlled by the extent of interaction of fillers with PVDF. Interestingly, both ß-lamellar morphology and degree of orientation correlate well with the mechanical properties of the rolled PVDF. More specifically, the dynamic storage modulus of the samples in the rolling direction increases with increasing ß-lamellar morphology and degree of orientation. The present work demonstrates that the polymer-filler interaction plays a crucial role in regulating the processed polymer morphology and can be tuned by appropriately modifying the surface of fillers through either covalent or non-covalent interactions.
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The same copper phosphate catalysts were synthesized by obtaining the methods involving solid state as well as liquid state reactions in this work. And then the optimised p-n hybrid junction photocatalysts have been synthesized following the same solid/liquid reaction pathways. The synthesized copper phosphate photocatalyst has unique rod, flower, caramel-treat-like morphology. The Mott-Schottky behavior is in accordance with the expected behavior of n-type semiconductor and the carrier concentration was calculated using the M-S analysis for the photocatalyst. And for the p-n hybrid junction of 8RGO-Cu3(PO4)2-PA (PA abbreviated for photoassisted synthesis method), 8RGO-Cu3(PO4)2-EG(EG abbreviated for Ethylene Glycol based synthesis method), 8RGO-Cu3(PO4)2-PEG (PEG abbreviated for Poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol based synthesis method)the amount of H2 synthesized was 7500, 6500 and 4500 µmol/h/g, respectively. The excited electrons resulting after the irradiation of visible light on the CB of p-type reduced graphene oxide (RGO) migrate easily to n-type Cu3(PO4)2 via. the p-n junction interfaces and hence great charge carrier separation was achieved.
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The present work demonstrates an extremely proficient and robust study of efficient interfacial charge transfer through plasmonic Ag decorated Bi2O3 hierarchical photoanodes for the photoelectrochemical treatment of chlorinated phenols. Unique 2D flake-like Bi2O3 hierarchical nanostructures were grown onto a fluorine-doped tin oxide (FTO) substrate by a simple chemical bath deposition method using triethanolamine as complexing agent. The formation of Bi2O3 on FTO was governed by the decomposition of a nucleated bismuth-hydroxyl complex (Bi2O1-x(OH)x) and modification to the electrode was carried out by the deposition of Ag via a chemical reduction method using hydrazine hydrate. Both the fabricated electrodes were well characterized for their photo- and electro-optical properties. Efficient charge separation was observed due to the surface plasmon resonance phenomenon of silver nanoparticles with the favorable intrinsic properties of Bi2O3 under application of a small electric bias of 1 V preventing the recombination of charge carriers and thereby increasing the rate of photoelectrocatalytic degradation of the chlorinated phenols. PEC degradation using the Ag@Bi2O3 photoelectrode followed the trend 4-CP < 2,4-DCP < 2,4,6-TCP < P-CP due to efficient attack at the chlorinated positions by reactive oxygen species with increasing chlorine substitution and also due to the absence of an expected chain reaction of the generated chlorine radicals (ClË) during the PEC reaction. The PEC activity of Ag@Bi2O3 was 1.5 times higher than a Bi2O3 nanoflake electrode for 4-CP over 2 h. The fabricated Ag@Bi2O3 proved to be an efficient photoelectrode with synergistic solar-induced photoactivity. A detailed mechanistic study in the presence of scavengers suggests degradation by produced hydroxyl radical species. Thus, physical insights into the degradation of chlorinated phenols were obtained.
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In the recent times, multifunctional materials have attracted immense interest. Self-healing polymers are in great demand in almost every coating application. With an increase in electromagnetic (EM) pollution, curbing the same has become an urgent necessity. Lightweight coatings and conducting polymeric materials are being highly researched upon in this regard, and combining these properties with self-healing systems would open new avenues in EM interference (EMI) shielding (specifically in the microwave frequency domain) applications. In the current study, a novel approach toward the development of microwave shielding materials capable of self-healing through microwave heating has been attempted. A covalently cross-linked material was developed using Diels-Alder (DA) chemistry, which shows self-healing properties when stimulated by heating. Herein, reduced graphene oxide grafted with magnetite nanoparticles (rGO/Fe3O4) was covalently cross-linked to thermoplastic polyurethane using DA chemistry. The addition of multiwalled carbon nanotubes into these nanocomposites led to exceptional EM wave shielding and self-healing properties through a synergistic effect. The synergism led to exceptional EMI shielding of -36 dB, primarily through absorption in the microwave region of the EM spectrum. When used in the form of thin coatings of about 1 mm in thickness, the shielding value reached -28 dB, manifesting in more than 99% attenuation of EM waves through absorption. The material was also found to be capable of healing scratches or cuts through microwave irradiation.
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A coatable polyvinylbutyral (PVB)-polyaniline (PANI) nanocomposite was designed for high microwave absorption efficiency. The maximum absorption efficiency 88.2 dB GHz/mm was obtained for the PANI nanofiber-loaded PVB (PVBPN) nanocomposite with a large bandwidth, whereas a pristine PANI-containing composite shows 53.5 dB GHz/mm in the frequency range 8.2-18 GHz. The presence of nanoslit pores in PVBPN also helps to achieve a large bandwidth and hence high microwave absorption efficiency. Standard electromagnetic simulation also shows that power absorbed by the PVBPN nanocomposite is high and its ultrathin coating over the dielectric substrate (epoxy) is promising for broadband tuneable reflection loss.
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Herein, graphene oxide (GO) was suitably functionalized to obtain carboxylated and fluorinated GO (GOCOOH and GOF) derivatives, respectively, via the Hunsdiecker reaction. Electrospun mats of poly(vinylidene fluoride) (PVDF)/GO, PVDF/GOCOOH, and PVDF/GOF fibers were then prepared by electrospinning from well-dispersed GO derivatives. The piezoelectric coefficient (d 33), as measured using piezoelectric force measurement (PFM), enhanced by more than 2 folds with respect to the control PVDF spun mat. The piezoelectric coefficient though enhanced upon the addition of GO and GOCOOH, however, enhanced significantly in the case of GOF. For instance, a drastic increase in piezoelectric response from 30 pm V-1(electrospun neat PVDF) to 63 pm V-1 (for electrospun PVDF/GOF) was observed as revealed from PFM results. The phase transformation in these fibers was systematically investigated by various techniques such as Fourier transform infrared spectroscopy (FTIR), wide angle X-ray diffraction (XRD), Raman spectroscopy, and PFM. FTIR and XRD results revealed that the electrospun fiber mats showed predominantly ß-PVDF. Interestingly, the highest ß content was obtained in the presence of GOF. The drastic enhancement in ß phase is due to the presence of highly electronegative fluorine. The addition of GOCOOH and GOF in PVDF not only increases the polar ß phase but also changes the piezoelectric response significantly. More interestingly, PVDF/GOF films exhibited higher energy density and dielectric permittivity when compared with the control PVDF samples. These findings will help guide the researchers working in this field from both theoretical understanding and practical view point for energy storing device and charge storage electronics.
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The present study elucidates the facile synthesis and exceptional properties of a family of novel poly(ester amide)s (PEAs) based on bis(2-hydroxy ethylene) terephthalamide that was obtained from the poly(ethylene terephthalate) waste. Fourier transform infrared and 1H NMR were used to verify the presence of ester and amide in the polymer backbone. Differential scanning calorimetry data showed that the glass transition temperature decreased with as the chain length of dicarboxylic acids increased. Dynamic mechanical analysis and contact angle studies proved that the modulus values and hydrophobicity increased with as the chain lengths of dicarboxylic acids increased. In vitro hydrolytic degradation and dye release studies demonstrated that the degradation and release decreased with as the chain lengths of dicarboxylic acids increased. Modeling these data illustrated that degradation and release follow first-order degradation and zero-order release, respectively. The in vitro cytocompatibility studies confirmed the minimal toxicity characteristic of these polymers. Osteogenic studies proved that these polymers can be highly influential in diverting the cells toward osteogenic lineage. Alizarin red staining evinced the presence of twice the amount of calcium phosphate deposits by the cells on these polymers when compared to the control. The observed result was also corroborated by the increased expression of alkaline phosphatase. These findings were further validated by the markedly higher mRNA expressions for known osteogenic markers using real time polymerase chain reaction. Therefore, these polymers efficiently promoted osteogenesis. This study demonstrates that the physical properties, degradation, and release kinetics can be altered to meet the specific requirements in organ regeneration as well as facilitate simultaneous polymer resorption through control of the chain length of the monomers. The findings of this study have significant implications for designing cost-effective biodegradable polymers for tissue engineering.
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Amidas/química , Materiais Biocompatíveis , Regeneração Óssea , Preparações de Ação Retardada , Etilenos , Ácidos Ftálicos , Poliésteres , PolietilenotereftalatosRESUMO
Polymeric architectures with controlled and well-defined structural features are required to render a sustainable antibacterial surface - a key requirement in the design of polymeric membranes for water purification. Herein, surface selective crosslinking of copper oxide-polyphosphoester (CuO-PPE) hybrid nanogels on to polyvinylidene fluoride-styrene maleic anhydride (PVDF/SMA) ultrafiltration membranes was developed. The hybrid nanogels, composed of PPE and CuO, with inherent antifouling and antibacterial properties, were crosslinked using a macroinitiator (polyethylene glycol, PEG) and subsequently grafted on to PVDF/SMA by alkyne-anhydride reaction. Partially hydrolysed SMA solubilizes membrane proteins and the phosphatase/phospholipase triggers the cleavage of PPE segments resulting in controlled release of Cu ions. This unique strategy renders the membrane surface antibacterial through sustained and controlled release of Cu ions thereby generating intracellular reactive oxygen species (ROS). In addition, the enhanced antibiofouling performance of these membranes is facilitated by the presence of the hydrophilic macroinitiator (PEG and PPE). The modified membranes designed in this study are durable and possess long-term stability due to strong covalent interaction between CuO-PPE and the PVDF/SMA membrane. Studies on the flux, porosity and protein adsorption of the membranes were performed. An enhanced flux recovery ratio was observed for the modified membrane due to the pendant PPE groups (from CuO-PPE) which prohibit irreversible protein adsorption on the PVDF surface. The cytotoxicity of CuO-PPE is greatly reduced because of an effective coverage of CuO by biocompatible PPEs. This study opens up new avenues of fabricating "smart" inorganic nanoparticles that can be confined in a soft hybrid polymeric gel network with controlled release of Cu ions thereby precluding ubiquitous bacterial treatment in water filtration systems.
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Biodiesel or fatty acid methyl esters (FAMEs) is primarily synthesized using edible vegetable oils and methanol with a catalyst. However, in the present study, FAMEs were synthesized from a non-edible oil (Calophyllum inophyllum also called as sura honne, Punnagam, Alexandrian Laurel) in different supercritical fluids: methanol (MeOH), methyl tert-butyl ether (MTBE), methyl acetate (MeOAc) and dimethyl carbonate (DMC) non-catalytically. Reactions were performed from 523K to 673K at 30MPa with a molar ratio of 40:1 with times varying from 3min to 3h. Conversions higher than 80% were obtained within 30min for oil reaction with MeOH and DMC at 623K and conversions of 60% and 70% were obtained at 673K with MeOAc and MTBE, respectively. Pseudo first order kinetics was used to obtain the rate constants and the activation energies followed the order: EMeOHAssuntos
Biocombustíveis
, Calophyllum
, Catálise
, Esterificação
, Metanol
, Éteres Metílicos
, Óleos de Plantas
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This work reports the synthesis of a novel, aspirin-loaded, linear poly (anhydride ester) and provides mechanistic insights into the release of aspirin from this polymer for anti-inflammatory activity. As compared to conventional drug delivery systems that rely on diffusion based release, incorporation of bioactives in the polymer backbone is challenging and high loading is difficult to achieve. In the present study, we exploit the pentafunctional sugar alcohol (xylitol) to provide sites for drug (aspirin) attachment at its non-terminal OH groups. The terminal OH groups are polymerized with a diacid anhydride. The hydrolysis of the anhydride and ester bonds under physiological conditions release aspirin from the matrix. The resulting poly(anhydride ester) has high drug loading (53%) and displays controlled release kinetics of aspirin. The polymer releases 8.5 % and 20%, of the loaded drug in one and four weeks, respectively and has a release rate constant of 0.0035h-0.61. The release rate is suitable for its use as an anti-inflammatory agent without being cytotoxic. The polymer exhibits good cytocompatibility and anti-inflammatory properties and may find applications as injectable or as an implantable bioactive material. The physical insights into the release mechanism can provide development of other drug loaded polymers.
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Anidridos/química , Anti-Inflamatórios/administração & dosagem , Aspirina/administração & dosagem , Preparações de Ação Retardada , Ésteres/química , Portadores de Fármacos/química , PolímerosRESUMO
Various classes of biodegradable polymers have been explored towards finding alternates for the existing treatments for bone disorders. In this framework, two families of polyesters using an array of crosslinkers were synthesized. One was based on galactiol/adipic acid and the other based on galactitol/dodecanedioic acid. The structures of the polymers were confirmed by FTIR and further confirmed by 1H NMR. DSC showed that the polymers were amorphous and the glass transition temperature increased with increase in crosslinking. DMA and contact angle analysis revealed that the modulus and hydrophobicity increased with increase in crosslinking. Swelling studies demonstrated that %swelling decreased with increase in crosslinking. The in vitro hydrolytic degradation studies and dye release studies of all the polymers exhibited that the degradation and release rate decreased with increase in crosslinking, hydrophobicity and modulus. Degradation and release followed first order kinetics and Higuchi kinetics, respectively. The preliminary in vitro cytotoxicity studies proved that this array of polymers was not cytotoxic. Osteogenic differentiation of pre-osteoblasts was observed in three dimensional (3D) porous scaffolds prepared using these polymers. This study demonstrates the ability to modulate the physical properties, degradation and release kinetics of these biodegradable polymers through smart selection of crosslinkers. The findings of these studies have important implications for developing novel biodegradable polymers for drug delivery and tissue engineering applications.