Search results for: functionalized zeolites

Authors: M. Rajabi, O. Moradi

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In this study, removal of Nickel and Zinc by graphene oxide and functionalized graphene oxide–gelaycin surfaces was examined. Amino group was added to surface of graphene oxide to produced functionalized graphene oxide–gelaycin. Effect of contact time and initial concentration of Ni (II) and Zn(II) ions were studied. Results showed that with increase of initial concentration of Ni (II) and Zn(II) adsorption capacity was increased. After 50 min has not a large change at adsorption capacity therefore, 50 min was selected as optimaze time. Scanning electron microscope (SEM) and fourier transform infrared (FT-IR) spectroscopy spectra used for the analysis confirmed the successful fictionalization of the Graphene oxide surface. Adsorption experiments of Ni (II) and Zn(II) ions graphene oxide and functionalized graphene oxide–gelaycin surfaces fixed at 298 K and pH=6. The Pseudo Firs-order and the Pseudo Second-order (types I, II, III and IV) kinetic models were tested for adsorption process and results showed that the kinetic parameters best fits with to type (I) of pseudo-second-order model because presented low X2 values and also high R2 values.

Keywords: graphene oxide, gelaycin, nickel, zinc, adsorption, kinetic, graphene oxide, gelaycin, nickel, zinc, adsorption, kinetic

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Authors: Prabhavathi Sundaram, Heidi Abrahamse

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In recent years, nanotechnology coupled with photodynamic therapy (PDT) has received considerable attention in terms of improving the effectiveness of drug delivery in cancer therapeutics. The development of functionalized single-walled carbon nanotubes (SWCNTs) has become revolutionary in targeted photosensitizers delivery since it improves the therapeutic index of drugs. The objective of this study was to prepare, characterize and evaluate the potential of functionalized SWCNTs using hyaluronic acid and loading it with photosensitizer and to effectively target colon cancer cells. The single-walled carbon nanotubes were covalently functionalized with hyaluronic acid and the loaded photosensitizer by non-covalent interaction. The photodynamic effect of SWCNTs is detected under laser irradiation in vitro. The hyaluronic acid-functionalized nanocomposites had a good affinity with CD44 receptors, and it avidly binds on to the surface of CACO-2 cells. The cellular uptake of nanocomposites was studied using fluorescence microscopy using lyso tracker. The anticancer activity of nanocomposites was analyzed in CACO-2 cells using different studies such as cell morphology, cell apoptosis, and nuclear morphology. The combined effect of nanocomposites and PDT improved the therapeutic effect of cancer treatment. The study suggested that the nanocomposites and PDT have great potential in the treatment of colon cancer.

Keywords: colon cancer, hyaluronic acid, single walled carbon nanotubes, photosensitizers, photodynamic therapy

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Authors: Shahryar Aftabi, Saeed Fathi, Mohammad H. Aminfar

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It is well known that cemented sand is one of the best approaches for soil stabilization. In some cases, a blend of sand, cement and other pozzolan materials such as zeolite, nano-particles and fiber can be widely (commercially) available and be effectively used in soil stabilization, especially in road construction. In this research, we investigate the effects of CaO which is based on the geotechnical characteristics of zeolite composition with sandy silt soil. Zeolites have low amount of CaO in their structures, that is, varying from 3% to 10%, and by removing the cement paste, we want to investigate the effect of zeolite pozzolan without any activator on soil samples strength. In this research, experiments are concentrated on various weight percentages of zeolite in the soil to examine the effect of the zeolite on drainage shear strength and California Bearing Ratio (CBR) both with and without curing. The study also investigates their liquid limit and plastic limit behavior and makes a comparative result by using Feng's and Wroth-Wood's methods in fall cone (cone penetrometer) device; in the final the SEM images have been presented. The results show that by increasing the percentage of zeolite in without-curing samples, the fine zeolite particles increase some soil's strength, but in the curing-state we can see a relatively higher strength toward without-curing state, since the zeolites have no plastic behavior, the pozzolanic property of zeolites plays a much higher role than cementing properties. Indeed, it is better to combine zeolite particle with activator material such as cement or lime to gain better results.

Keywords: California bearing ratio, CBR, direct shear, fall-cone, sandy silt, SEM, zeolite

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Authors: Surjyakanta Rana, Sreekantha B. Jonnalagadda

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Synthesis of well distributed Pd nanoparticles (3 – 7 nm) on organo amine-functionalized graphene is reported, which demonstrated excellent catalytic activity towards Suzuki coupling reaction. The active material was characterized by X-ray diffraction (XRD), BET surface area, X-ray photoelectron spectra (XPS), Fourier-transfer infrared spectroscopy (FTIR), Raman spectra, Scanning electron microscope (SEM), Transmittance electron microscopy (TEM) analysis and HRTEM. FT-IR revealed that the organic amine functional group was successfully grafted onto the graphene oxide surface. The formation of palladium nanoparticles was confirmed by XPS, TEM and HRTEM techniques. The catalytic activity in the coupling reaction was superb with 100% conversion and 98 % yield and also activity remained almost unaltered up to six cycles. Typically, an extremely high turnover frequency of 185,078 h-1 is observed in the C-C Suzuki coupling reaction using organo di-amine functionalized graphene as catalyst.

Keywords: Di-amine, graphene, Pd nanoparticle, suzuki coupling

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Authors: Said M. AL-Mashaikhi, El-Said I. El-Shafey, Fakhreldin O. Suliman, Saleh Al-Busafi

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Activated carbon (AC) was prepared from date palm leaflets via NaOH activation. AC was oxidized using nitric acid, producing oxidized activated carbon (OAC). OAC was surface functionalized using different amine surfactants, including methylamine (ONM), ethylamine (ONE), and diethylamine (ONDE) using the amide coupling process. Produced carbons were surface characterized for surface area and porosity, X-ray diffraction, SEM, FTIR, and TGA. AC surface area (580 m²/g) has shown a decrease in oxidation to 260 m²/g for OAC. On amine functionalization, the surface area has further decreased to 218, 108, and 20 m²/g on functionalization with methylamine, ethylamine, and diethylamine, respectively. FTIR and TGA showed that the nature of amine functionalization of AC is chemical. Methylene blue sorption was tested on these carbons in terms of kinetics and equilibrium. Sorption was found faster on amine-functionalized carbons than both AC and OAC, and this is due to hydrophobic interaction with the alkyl groups immobilized with data following pseudo second-order reaction. On the other hand, AC showed the slowest adsorption kinetic process due to the diffusion in the porous structure of AC. Sorption equilibrium data was found to follow the Langmuir sorption isotherm with maximum sorption found on ONE. Regardless of its lower surface area than activated carbon, ethylamine functionalized AC showed better performance than AC in terms of kinetics and equilibrium for dye removal.

Keywords: activated carbon, dye removal, functionalization, hydrophobic interaction, water treatment

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Authors: D. A. Bruzon, G. Tapang, I. S. Martinez

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Global warming and climate change are significant environmental concerns, which require immediate global action in carbon emission mitigation. The capture, sequestration, and conversion of carbon dioxide to other products such as methane or ethanol are ways to control excessive emissions. Ionic liquids have shown great potential among the materials studied as carbon capture solvents and catalysts in the reduction of CO2. In this study, ionic liquids comprising of a methoxy (-OCH3) and cyano (-CN) functionalized imidazolium cation, [MOBMIM] and [CNBMIM] respectively, paired with tris(pentafluoroethyl)trifluorophosphate [FAP] anion were evaluated as effective capture solvents, and organocatalysts in the reduction of CO2. An in-situ electrochemical set-up, which can measure controlled amounts of CO2 both in the gas and in the ionic liquid phase, was used. Initially, reduction potentials of CO2 in the CO2-saturated ionic liquids containing the internal standard cobaltocene were determined using cyclic voltammetry. Chronoamperometric transients were obtained at potentials slightly less negative than the reduction potentials of CO2 in each ionic liquid. The time-dependent current response was measured under a controlled atmosphere. Reduction potentials of CO2 in methoxy and cyano-functionalized [FAP] ionic liquids were observed to occur at ca. -1.0 V (vs. Cc+/Cc), which was significantly lower compared to the non-functionalized analog [PMIM][FAP], with an observed reduction potential of CO2 at -1.6 V (vs. Cc+/Cc). This decrease in the potential required for CO2 reduction in the functionalized ionic liquids shows that the functional groups methoxy and cyano effectively decreased the free energy of formation of the radical anion CO2●⁻, suggesting that these electrolytes may be used as organocatalysts in the reduction of the greenhouse gas. However, upon analyzing the solubility of the gas in each ionic liquid, [PMIM][FAP] showed the highest absorption capacity, at 4.81 mM under saturated conditions, compared to [MOBMIM][FAP] at 1.86 mM, and [CNBMIM][FAP] at 0.76 mM. Also, calculated Henry’s constant determined from the concentration-pressure graph of each functionalized ionic liquid shows that the groups -OCH3 and -CN attached terminal to a C4 alkyl chain do not significantly improve CO2 solubility.

Keywords: carbon capture, CO2 reduction, electrochemistry, ionic liquids

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Authors: K. Menad, A. Feddag, M. A. Hassnaoui

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We are living in a time and in a world heavily polluted. In the list of the great dangers awaiting the man can be placed on top of the list pollution by heavy metals: lead, mercury, cadmium, etc. Fatigue, Depression, Thyroid disorder, Alzheimer's, Parkinson's, Cancer, are some of the health problems caused by heavy metal pollution. The environmental protection has long since become a major political and economic issue. Among the priorities, include safeguarding water resources. All countries of the world are concerned either because they lack water or because they pollute it. There are several ways to remove these heavy metals; ion exchange by zeolites is one of these ways, which our work is based on. Zeolites were among the main clean up materials by either adsorption, ion exchange and catalysis. Lead and cadmium, heavy metals, is one of the main dangers fulminate the flora and fauna of our small planet, so many resources are deployed to remedy them. The elimination of lead and cadmium by ion exchange has been extensively studied. However, exchange capacity of more and larger formed a major challenge for researchers and industry.

Keywords: composite, ion excahnge, zeolite LTA, zeolite x

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Authors: Morteza Keshavarz

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In this work, using density functional theory (DFT) thermodynamic stability and quantum molecular descriptors of cyclophoshphamide (an anticancer drug)-functionalized zigzag (8,0) CNT, armchair (4,4) CNT and nanocone complexes in water, for two attachment namely the sidewall and tip, is considered. Calculation of the total electronic energy (Et) and binding energy (Eb) of all complexes indicates that the most thermodynamic stability belongs to the sidewall-attachment of cyclophosphamide into functional nanocone. On the other hand, results from chemical hardness show that drug-functionalized zigzag (8,0) and armchair (4,4) complexes in the tip-attachment configuration possess the smallest and greatest chemical hardness, respectively. By computing the solvation energy, it is found that the solution of the drug and all complexes are spontaneous in water. Furthermore, chirality, type of nanovector (nanotube or nanocone), or attachment configuration have no effects on solvation energy of complexes.

Keywords: carbon nanotube, drug delivery, cyclophosphamide drug, density functional theory (DFT)

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Authors: Gina Zavaleta-Espejo, Segundo R. Jáuregui-Rosas, Fanny V. Samanamud-Moreno, José Saldaña Jiménez, Anibal Felix-Quintero, Víctor Montero-Del Aguila, Elsi Mejía-Uriarte

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Vicugnapacos "alpaca" fabrics are considered special for their finesse, and the garments in the textile market are very luxurious. It has many special characteristics such as antiallergic, soft, hygroscopic, among others. In this sense, the research aimed to evaluate the antimicrobial activity of alpaca fabrics functionalized with silver nanoparticles on the bacteria Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 25923. For the functionalization of the fabrics, AgNO3 and different concentrations of trisodium citrate (TSC) 2, 6, and 10 mg. Tissue characterization was performed using Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The determination of the antimicrobial activity of the alpaca tissues was made by the Kirby-Bauer method with alpaca tissue discs functionalized with silver nanoparticles, an experimental design was made in completely randomized blocks with three treatments and a negative control with three repetitions. The results showed that inhibition halos were formed for both bacteria, therefore, the functionalized tissues have a high antimicrobial activity, whose mechanism of action is attributed to the free radicals (ROS) generated by the nanoparticles that cause oxidative damage to the bacteria. proteins and lipids of the bacterial cell wall.

Keywords: antimicrobial, animal fibers, fabrics, functionalization, trisodium citrate

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Authors: Yongjun Ahn, Sung Gyu Choi, Seung-Yeop Kwak

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Selective removal of free fatty acid (FFA) and chlorophyll in extra virgin olive oil (EVOO) is necessary to enhance the thermal stability in the condition of the deep frying. In this work, we demonstrated improving the thermal stability of EVOO by selective removal of free fatty acid and chlorophyll using (3-Aminopropyl)trimethoxysilane (APTMS) functionalized mesoporous silica with controlled pore size. The adsorption kinetics of free fatty acid and chlorophyll into the mesoporous silica were quantitatively analyzed by Freundlich and Langmuir model. The highest chlorophyll adsorption efficiency was shown in the pore size at 5 nm, suggesting that the interaction between the silica and the chlorophyll could be optimized at this point. The amino-functionalized mesoporous silica showed drastically improved removal efficiency of FFA than the bare silica. Moreover, beneficial compounds like tocopherol and phenolic compounds maintained even after adsorptive removal. Extra virgin olive oil treated by aminopropyl-functionalized silica had a smoke point high enough to be used as commercial frying oil. Based on these results, it is expected to attract the considerable amount of interest toward facile adsorptive refining process of EVOO using pore size controlled and amino-functionalized mesoporous silica.

Keywords: mesoporous silica, extra virgin olive oil, selective adsorption, thermal stability

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Authors: Homa Torabizadeh, Mohaddeseh Mikani

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Inulinase from Aspergillus niger was covalently immobilized on magnetic nanoparticles (MNPs/Fe₃O₄) covered with soy protein isolate (SPI/Fe₃O₄) functionalized by bovine serum albumin (BSA) nanoparticles. MNPs are promising enzyme carriers because they separate easily under external magnetic fields and have enhanced immobilized enzyme reusability. As MNPs aggregate simply, surface coating strategy was employed. SPI functionalized by BSA was a suitable candidate for nanomagnetite coating due to its superior biocompatibility and hydrophilicity. Fe₃O₄@SPI-BSA nanoparticles were synthesized as a novel carrier with narrow particle size distribution. Step by step fabrication monitoring of Fe₃O₄@SPI-BSA nanoparticles was performed using field emission scanning electron microscopy and dynamic light scattering. The results illustrated that nanomagnetite with the spherical morphology was well monodispersed with the diameter of about 35 nm. The average size of the SPI-BSA nanoparticles was 80 to 90 nm, and their zeta potential was around −34 mV. Finally, the mean diameter of fabricated Fe₃O₄@SPI-BSA NPs was less than 120 nm. Inulinase enzyme from Aspergillus niger was covalently immobilized through gluteraldehyde on Fe₃O₄@SPI-BSA nanoparticles successfully. Fourier transform infrared spectra and field emission scanning electron microscopy images provided sufficient proof for the enzyme immobilization on the nanoparticles with 80% enzyme loading.

Keywords: high fructose syrup, inulinase immobilization, functionalized magnetic nanoparticles, soy protein isolate

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Authors: P. D. Ibikunle, D. O. Bala, A. P. Olawolu, A. A. Adebayo

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Chromium has been discovered as a significant contributor to water pollution that causes cancer. Modified carbon nanotubes' (CNTs) potential as an adsorbent hasn't been thoroughly investigated. The study aimed at investigating the potentials of various functionalized carbon nanomaterials for Cr (VI) removal from contaminated synthetic groundwater. Functionalized carbon nanomaterials with layered and tube-like structures were designed based on thermal (KOH-activated micrographite sheets) and impregnation methods by anchoring K and Zn on carbon nanotubes (CNTs), respectively for the removal of Cr (VI) from contaminated synthetic groundwater. Zinc acetate modified carbon nanotubes (Zn-CNTs) and potassium hydroxide modified carbon nanotubes (K-CNTs) exhibited greater adsorption capacity for the Cr (VI) adsorbate compared to KOH-activated graphite (AC-1 and AC-0). Maximum removal efficiency for both adsorbents occurred at pH 2. Omu Aran Hand dug wells can therefore be treated with K–CNTs, since the experimental outcomes showed that CNTs adsorbent could operate well in a range of the experimental scenarios.

Keywords: carbon nanotubes, Chromium (VI), adsorption, water treatment, graphitic carbon, kinetics

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Authors: Karen G. Bastidas Gomez, Hugo R. Zea Ramirez, Manuel F. Ribeiro Pereira, Cesar A. Sierra Avila, Juan A. Clavijo Morales

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The contamination of water sources with heavy metals such as mercury has been an environmental problem; it has generated a high impact on the environment and human health. In countries such as Colombia, mercury contamination due to mining has reached levels much higher than the world average. This work proposes the use of fique fibers as adsorbent in mercury removal. The evaluation of the material was carried out under five different conditions (raw, pretreated by organosolv, functionalized by TEMPO oxidation, fiber functionalized plus MOF-199 and fiber functionalized plus MOF-199-SH). All the materials were characterized using FTIR, SEM, EDX, XRD, and TGA. Regarding the mercury removal, it was done under room pressure and temperature, also pH = 7 for all materials presentations, followed by Atomic Absorption Spectroscopy. The high cellulose content in fique is the main particularity of this lignocellulosic biomass since the degree of oxidation depends on the number of hydroxyl groups on the surface capable of oxidizing into carboxylic acids, a functional group capable of increasing ion exchange with mercury in solution. It was also expected that the impregnation of the MOF would increase the mercury removal; however, it was found that the functionalized fique achieved a greater percentage of removal, resulting in 81.33% of removal, 44% for the fique with the MOF-199 and 72% for the MOF-199-SH with. The pretreated fiber and raw also showed 74% and 56%, respectively, which indicates that fique does not require considerable modifications in its structure to achieve good performances. Even so, the functionalized fiber increases the percentage of removal considerably compared to the pretreated fique, which suggests that the functionalization process is a feasible procedure to apply with the purpose of improving the removal percentage. In addition, this is a procedure that follows a green approach since the reagents involved have low environmental impact, and the contribution to the remediation of natural resources is high.

Keywords: biomass, nanotechnology, science materials, wastewater treatment

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Authors: Mumuni Sumaila, Viness Pillay, Yahya E. Choonara, Pradeep Kumar, Pierre P. Kondiah

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Tuberculosis (TB) remains a serious challenge to public health globally, despite every effort put together to curb the disease. Current TB therapeutics available have proven to be inefficient due to a multitude of drawbacks that range from serious adverse effects/drug toxicity to inconsistent bioavailability, which ultimately contributes to the emergence of drug-resistant TB. An effective ‘cargo’ system designed to cleverly deliver therapeutic doses of anti-TB drugs to infection sites and in a sustained-release manner may provide a better therapeutic choice towards winning the war against TB. In the current study, we investigated mannose-functionalized lipopolysaccharide hybrid nanoparticles for safety and efficacy towards macrophage-targeted simultaneous delivery of the two first-line anti-TB drugs, rifampicin (RF) and isoniazid (IS). RF-IS-loaded lipopolysaccharide hybrid nanoparticles were fabricated using the solvent injection technique (SIT), incorporating soy lecithin (SL) and low molecular weight chitosan (CS) as the lipid and polysaccharide components, respectively. Surface-functionalized nanoparticles were obtained through the reaction of the aldehyde group of mannose with free amine functionality present at the surface of the nanoparticles. The functionalized nanocarriers were spherical with average particle size and surface charge of 107.83 nm and +21.77 mV, respectively, and entrapment efficiencies (EE) were 53.52% and 69.80% for RF and IS, respectively. FTIR spectrum revealed high-intensity bands between 1663 cm⁻¹ and 1408 cm⁻¹ wavenumbers (absent in non-functionalized nanoparticles), which could be attributed to the C=N stretching vibration produced by the formation of Schiff’s base (–N=CH–) during the mannosylation reaction. In vitro release studies showed a sustained-release profile for RF and IS, with less than half of the total payload released over a 48-hour period. The nanocarriers were biocompatible and safe, with more than 80% cell viability achieved when incubated with RAW 264.7 cells at concentrations 30 to 500 μg/mL over a 24-hour period. Cellular uptake studies (after a 24-hour incubation period with the murine macrophage cells, RAW 264.7) revealed a 13- and a 9-fold increase in intracellular accumulation of RF and IS, respectively, when compared with the unformulated RF+IS solution. A 6- and a 3-fold increase in intracellular accumulation of RF and IS, respectively, were observed when compared with the non-functionalized nanoparticles. Furthermore, fluorescent microscopy images showed nanoparticle internalization and accumulation within the RAW 264.7 cells, which was more significant in the mannose-functionalized system compared to the non-functionalized nanoparticles. The overall results suggested that the fabricated mannose-functionalized lipopolysaccharide nanoparticles are a safe and promising platform for macrophage-targeted delivery of anti-TB therapeutics. However, in vivo pharmacokinetic/pharmacodynamics studies are required to further substantiate the therapeutic efficacy of the nanosystem.

Keywords: anti-tuberculosis therapeutics, hybrid nanosystem, lipopolysaccharide nanoparticles, macrophage-targeted delivery

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Authors: Lenka Matulova

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Geopolymers are alumosilicate materials that have long been studied. Despite this fact, little is known about the long-term stability of geopolymer mechanical and structural properties, so crucial for their successful industrial application. To improve understanding, we investigated the effect of four different types of environments on the mechanical and structural properties of a metakaolin-based geopolymer (MK GP). The MK GP samples were stored in laboratory conditions (control samples), in water at 20 °C, in water at 80 °C, and outside exposed to the weather. Compressive and tensile strengths were measured after 28, 56, 90, and 360 days. In parallel, structural properties were analyzed using XRD, SEM, and mercury intrusion porosimetry. Whereas the mechanical properties of the samples in laboratory conditions and in 20 °C water were stable, the mechanical properties of the outdoor samples and the samples 80 °C water decreased noticeably after 360 days. Structural analyses were focused on changes in sample microstructure (developing microcrack network, porosity) and identifying zeolites, the presence of which would indicate detrimental processes in the structure that can change it from amorphous to crystalline. No zeolites were found during the 360-day period in MK GP samples, but the reduction in mechanical properties coincided with a developing network of microcracks and changes in pore size distribution.

Keywords: geopolymer, long-term properties, mechanical properties, metakaolin, structural properties

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Authors: Ali Mohammed Yimer, Ayalew H. Assen, Youssef Belmabkhout

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This study delves into sustainable approaches for valorizing phosphatic wastes, specifically phosphate mining wastes and phosphogypsum, which are byproducts of phosphate industries and pose significant environmental challenges due to their accumulation. We propose a unified strategic synthesis method aimed at converting these wastes into hetero-functional porous materials. Our approach involves isolating the primary components of phosphatic wastes, such as CaO, SiO2 and Al2O3 to fabricate functional porous materials falling into two distinct classes. Firstly, alumina and silica components are extracted or isolated to produce zeolites (including CAN, GIS, SOD, FAU, and LTA), characterized by a Si/Al ratio of less than 5. Secondly, residual calcium is utilized to synthesize calcium-based metal–organic frameworks (Ca-MOFs) employing various organic linkers like Ca-BDC, Ca-BTC and Ca-TCPB (SBMOF-2), thereby providing flexibility in material design. Characterization techniques including XRD, SEM-EDX, FTIR, and TGA-MS affirm successful material assembly, while sorption analyses using N2, CO2, and H2O demonstrate the porosity of the materials. Particularly noteworthy is the water/alcohol separation potential exhibited by the Ca-BTC MOF, owing to its optimal pore aperture size (∼3.4 Å). To enhance replicability and scalability, detailed protocols for each synthesis step and specific conditions for each process are provided, ensuring that the methodology can be easily reproduced and scaled up for industrial applications. This synthetic transformation approach represents a valorization route for converting phosphatic wastes into extended porous structures, promising significant environmental and economic benefits.

Keywords: calcium-based metal-organic frameworks, low-silica zeolites, porous materials, sustainable synthesis, valorization

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Authors: Yu Wang, Xibang Chen, Maolin Zhai, Jing Peng, Jiuqiang Li

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Poly(acrylic acid) (PAA) functionalized magnetic graphene oxide (GO) composite was synthesized through a two-step process. Magnetic Fe₃O₄/GO was first prepared by a facile hydrothermal method. A radiation-induced grafting technique was used to graft PAA to Fe₃O₄/GO to obtain the Fe₃O₄/GO-g-PAA subsequently. The characteristics results of FTIR, Raman, XRD, SEM, TEM, and VSM showed that Fe₃O₄/GO-g-PAA was successfully prepared. The Fe₃O₄/GO-g-PAA composites were used as sorbents for the removal of Pb(II) ions, and the maximum adsorption capacity for Pb(II) was 176.92 mg/g.

Keywords: Fe₃O₄, graphene oxide, magnetic, Pb(II) removal, radiation-induced

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Authors: Prajakta Katti, Suryasarathi Bose, S. Kumar

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In this work, carboxyl functionalized multiwall carbon nanotubes (a-MWNTs) covalently grafted with hydroxylated functionalized poly (ether ether ketone), HPEEK, which is miscible with the pre-polymer (epoxy) through the esterification reaction. The functionalized MWNTs were systematically characterized using spectroscopic techniques. The epoxy composites containing a-MWNTs and HPEEK grafted multiwall carbon nanotubes (HPEEK-g-MWNTs) were formulated using mechanical stirring coupled with a bath sonicator to improve the dispersion property of the nanoparticles and were subsequently cured at 80 ̊C and post cured at 180 ̊C. With the addition of 0.5 wt% of HPEEK-g-MWNTs, an impressive 44% enhancement in the storage modulus, 22% increase in tensile strength and 38% increase in fracture toughness was observed with respect to neat epoxy. In addition to these mechanical properties, the epoxy composites displayed significant enhancement in the hardness without reducing thermal stability. These improved properties were attributed to the tailored interface between HPEEK-MWNTs and epoxy matrix.

Keywords: epoxy, MWNTs, HPEEK-g-MWNTs, tensile properties, nanoindentation, fracture toughness

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Authors: Rawaz A. Ahmed, Katherine Huddersman

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High-lipid Fats, Oils and Grease (FOGs) from wastewater are underutilized despite their potential for conversion into valuable fuels; this work describes a surface-functionalized fibrous Polyacrylonitrile (PAN) mesh as a novel heterogeneous acid catalyst for the conversion of free fatty acids (FFAs), via a catalytic esterification process into biodiesel. The esterification of stearic acid (SA) with methanol was studied over an acidified PAN solid acid catalyst. Disappearance of the carboxylic acid (C=O) peak of the stearic acid at 1696 cm-1 in the FT-IR spectrum with the associated appearance of the ester (C=O) peak at 1739 cm-1 confirmed the production of the methyl stearate. This was further supported by 1H NMR spectra with the appearance of the ester (-CH₂OCOR) at 3.60-3.70 ppm. Quantitate analysis by GC-FID showed the catalyst has excellent activity with >95 % yield of methyl stearate (MS) at 90 ◦C after 3 h and a molar ratio of methanol to SA of 35:1. To date, to our best knowledge, there is no research in the literature on the esterification reaction for biodiesel production using a modified PAN mesh as a catalyst. It is noteworthy that this acidified PAN mesh catalyst showed comparable activity to conventional Brönsted acids, namely H₂SO₄ and p-TSA, as well as exhibiting higher activity than various other heterogeneous catalysts such as zeolites, ion-exchange resins and acid clay.

Keywords: fats oil and greases (FOGs), free fatty acid, esterification reaction, methyl ester, PAN

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Authors: Mohannad N. H. Al-Malichi

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Because of its exceptional properties, graphene has become the most promising nanomaterial for the development of a new generation of advanced materials from battery electrodes to structural composites. However, current methods to meet requirements for the mass production of high-quality graphene are limited by harsh oxidation, high temperatures, and tedious processing steps. To extend the scope of the bulk production of graphene, herein, a facile, reproducible and cost-effective approach has been developed. This involved heating a specific mixture of chemical materials at an extremely low temperature (70 C) for a short period (7 minutes) to exfoliate functionalized graphene platelets with high structural integrity. The obtained graphene platelets have an average thickness of 3.86±0.71 nm and a lateral size less than ~2 µm with a low defect intensity ID/IG ~0.06. The thin film (~2 µm thick) exhibited a low surface resistance of ~0.63 Ω/sq⁻¹, confirming its high electrical conductivity. Additionally, these nanoplatelets were decorated with polar functional groups (epoxy and carboxyl groups), thus have the potential to toughen and provide multifunctional polymer nanocomposites. Moreover, such a simple method can be further exploited for the novel exfoliation of other layered two-dimensional materials such as MXenes.

Keywords: functionalized graphene nanoplatelets, high structural integrity graphene, low temperature exfoliation of graphene, functional graphene platelets

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Authors: Ghodsieh Isapour Toutizad, Aiyong Wang, Joonsoo Han, Derek Creaser, Louise Olsson, Magnus Skoglundh, Hanna HaRelind

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Nitrous oxide (N2O), which is generally formed as a byproduct of industrial chemical processes and fossil fuel combustion, has attracted considerable attention due to its destructive role in global warming and ozone layer depletion. From various developed technologies used for lean NOx reduction, the selective catalytic reduction (SCR) of NOx with ammonia is presently the most applied method. Therefore, the development of catalysts for efficient lean NOx reduction without forming N2O in the process, or only forming it to a very small extent from the exhaust gases is of crucial significance. One type of catalysts that nowadays are used for this aim are zeolite-based catalysts. It is owing to their remarkable catalytic performance under practical reaction conditions such as high thermal stability and high N2 selectivity. Among all zeolites, copper ion-exchanged zeolites, with CHA, MFI, and BEA framework structure (like SSZ-13, ZSM-5 and Beta, respectively), represent higher hydrothermal stability, high activity and N2 selectivity. This work aims at investigating the effect of the zeolite framework structure on the formation of N2O during NH3-SCR reaction conditions over three Cu-based zeolites ranging from small-pore to large-pore framework structure. In the zeolite framework, Cu exists in two cationic forms, that can catalyze the SCR reaction by activating NO to form NO+ and/or surface nitrate species. The nitrate species can thereafter react with NH3 to form another intermediate, ammonium nitrate, which seems to be one source for N2O formation at low temperatures. The results from in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) indicate that during the NO oxidation step, mainly NO+ and nitrate species are formed on the surface of the catalysts. The intensity of the absorption peak attributed to NO+ species is higher for the Cu-CHA sample compared to the other two samples, indicating a higher stability of this species in small cages. Furthermore, upon the addition of NH3, through the standard SCR reaction conditions, absorption peaks assigned to N-H stretching and bending vibrations are building up. At the same time, negative peaks are evolving in the O-H stretching region, indicating blocking/replacement of surface OH-groups by NH3 and NH4+. By removing NH3 and adding NO2 to the inlet gas composition, the peaks in the N-H stretching and bending vibration regions show a decreasing trend in intensity, with the decrease being more pronounced for increasing pore size. It can probably be owing to the higher accumulation of ammonia species in the small-pore size zeolite compared to the other two samples. Furthermore, it is worth noting that the ammonia surface species are strongly bonded to the CHA zeolite structure, which makes it more difficult to react with NO2. To conclude, the framework structure of the zeolite seems to play an important role in the formation and reactivity of surface species relevant for the SCR process. Here we intend to discuss the connection between the zeolite structure, the surface species, and the formation of N2O during ammonia-SCR.

Keywords: fast SCR, nitrous oxide, NOx, standard SCR, zeolites

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Authors: Meenakshi Verma, Mandeep Singh Bakshi, Kultar Singh

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Magnetic nanoparticles have received incredible importance in view of their diverse applications, which arise primarily due to their response to the external magnetic field. The magnetic behaviour of magnetic nanoparticles (NPs) helps them in numerous different ways. The most important amongst them is the ease with which they can be purified and also can be separated from the media in which they are present merely by applying an external magnetic field. This exceptional ease of separation of the magnetic NPs from an aqueous media enables them to use for extracting/removing metal pollutants from complex aqueous medium. Functionalized magnetic NPs can be subjected for the metallic impurities extraction if are favourably adsorbed on the NPs surfaces. We have successfully used the magnetic NPs as vehicles for gold and silver NPs removal from the complex fluids. The NPs loaded with gold and silver NPs pollutant fractions has been easily removed from the aqueous media by using external magnetic field. Similarly, we have used the magnetic NPs for extraction of protein from complex media and then constantly washed with pure water to eliminate the unwanted surface adsorbed components for quantitative estimation. The purified and protein loaded magnetic NPs are best analyzed with SDS Page to not only for characterization but also for separating the protein fractions. A collective review of the results indicates that we have synthesized surfactant coated iron oxide NPs and then functionalized these with selected materials. These surface active magnetic NPs work very well for the extraction of metallic NPs from the aqueous bulk and make the whole process environmentally sustainable. Also, magnetic NPs-Au/Ag/Pd hybrids have excellent protein extracting properties. They are much easier to use in order to extract the magnetic impurities as well as protein fractions under the effect of external magnetic field without any complex conventional purification methods.

Keywords: magnetic nanoparticles, protein, functionalized, extraction

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Authors: Roghaye Behroozi

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The development of functionalized metal complexes and nanomaterials has gained significant attention due to their potential in catalyzing selective oxidation and coupling reactions. These catalysts play a crucial role in various industrial and pharmaceutical processes, enhancing the efficiency, selectivity, and sustainability of chemical reactions. This research aims to design and synthesize new functionalized metal complexes and nanomaterials to explore their catalytic applications in the selective oxidation of alcohols and coupling reactions, focusing on improving yield, selectivity, and catalyst reusability. The study involves the synthesis of a nickel Schiff base complex stabilized within 41-MCM as a heterogeneous catalyst. A Schiff base ligand derived from glycine was used to create a tin (IV) metal complex characterized through spectroscopic techniques and computational analysis. Additionally, iron-based magnetic nanoparticles functionalized with melamine were synthesized for catalytic evaluation. Lastly, a palladium (IV) complex was prepared, and its oxidative stability was analyzed. The nickel Schiff base catalyst showed high selectivity in converting primary and secondary alcohols to aldehydes and ketones, with yields ranging from 73% to 90%. The tin (IV) complex demonstrated accurate structural and electronic properties, with consistent results between experimental and computational data. The melamine-functionalized iron nanoparticles exhibited efficient catalytic activity in producing triazoles, with enhanced reaction speed and reusability. The palladium (IV) complex displayed remarkable stability and low reactivity towards C–C bond formation due to its symmetrical structure. The synthesized metal complexes and nanomaterials demonstrated significant potential as efficient, selective, and reusable catalysts for oxidation and coupling reactions. These findings pave the way for developing environmentally friendly and cost-effective catalytic systems for industrial applications.

Keywords: catalysts, Schiff base complexes, metal-organic frameworks, oxidation reactions, nanoparticles, reusability

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Authors: Yi-Jie Lin, Jyh-Cherng Chen

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The fly ash of waste incineration processes is usually hazardous and the disposal or reuse of waste incineration fly ash is difficult. In this study, the waste incineration fly ash was converted to useful zeolites by the alkali fusion and hydrothermal synthesis method. The influence of different operating conditions (the ratio of Si/Al, the ratio of hydrolysis liquid to solid, and hydrothermal time) was investigated to seek the optimum operating conditions for the synthesis of zeolite from waste incineration fly ash. The results showed that concentrations of heavy metals in the leachate of Toxicity Characteristic Leaching Procedure (TCLP) were all lower than the regulatory limits except lead. The optimum operating conditions for the synthesis of zeolite from waste incineration fly ash by the alkali fusion and hydrothermal synthesis method were Si/Al=40, NaOH/ash=1.5, alkali fusion at 400 ^oC for 40 min, hydrolysis with Liquid to Solid ratio (L/S)= 200 at 105 ^oC for 24 h, and hydrothermal synthesis at 105 ^oC for 24 h. The specific surface area of fly ash could be significantly increased from 8.59 m²/g to 651.51 m²/g (synthesized zeolite). The influence of different operating conditions on the synthesis of zeolite from waste incineration fly ash followed the sequence of Si/Al ratio > hydrothermal time > hydrolysis L/S ratio. The synthesized zeolites can be reused as good adsorbents to control the air or wastewater pollutants. The purpose of fly ash detoxification, reduction and waste recycling/reuse is achieved successfully.

Keywords: alkali fusion, hydrothermal, fly ash, zeolite

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Authors: Dinda A. Utami, Muhammad N. Alfarizi

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The purpose of this study was to determine the ability of zeolite catalyst for the trans- esterification reaction in biodiesel production from animal fat. The ability of the zeolite as a catalyst is determined by the structure and composition of the zeolite. An important factor that determines the properties of zeolites in catalysis includes adsorption capability to the compound of the reactants. Zeolites with a pore size of specific properties selectively adsorbing molecules. A molecule can be adsorbed by either the zeolite cavities if the size and shape of the molecule in accordance with the size and shape of the cavity in the zeolite. At this time, it is common to use homogeneous catalysts for biodiesel. We know these catalysts have some disadvantages in its use. Such as the difficulty of separation of the product with the catalyst, the generation of waste that is harmful to the environment due to residual catalysts can’t be reused, and the difficulty of handling and storage. But nowadays, solid catalyst developed technically to improve the efficiency of biodiesel production. In this case of study, we used trans-esterification process wherein the triglyceride is reacted with an alcohol with zeolite as a solid catalyst and it will produce biodiesel and glycerol as a byproduct. Development of solid catalyst seems to be the perfect solution to address the problems associated with homogeneous catalysts.

Keywords: biodiesel, animal fat, trans esterification, zeolite catalyst

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Authors: Mohamed Edokali, Robert Menzel, David Harbottle, Ali Hassanpour

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Forward osmosis (FO) process has stood out as an energy-efficient technology for water desalination and purification, although the practical application of FO for desalination still relies on RO-based Thin Film Composite (TFC) and Cellulose Triacetate (CTA) polymeric membranes which have a low performance. Recently, graphene oxide (GO) laminated membranes have been considered an ideal selection to overcome the bottleneck of the FO-polymeric membranes owing to their simple fabrication procedures, controllable thickness and pore size and high water permeability rates. However, the low stability of GO laminates in wet and harsh environments is still problematic. The recent developments of modified GO and hydrophobic reduced graphene oxide (rGO) membranes for FO desalination have demonstrated attempts to overcome the ongoing trade-off between desalination performance and stability, which is yet to be achieved prior to the practical implementation. In this study, acid-functionalized GO nanosheets cooperatively reduced and crosslinked by the hyperbranched polyethyleneimine (PEI) and polyethylene glycol (PEG) polymers, respectively, are applied for fabrication of the FO membrane, to enhance the membrane stability and performance, and compared with other functionalized rGO-FO membranes. PEI/PEG doped rGO membrane retained two compacted d-spacings (0.7 and 0.31 nm) compared to the acid-functionalized GO membrane alone (0.82 nm). Besides increasing the hydrophilicity, the coating layer of PEG onto the PEI-doped rGO membrane surface enhanced the structural integrity of the membrane chemically and mechanically. As a result of these synergetic effects, the PEI/PEG doped rGO membrane exhibited a water permeation of 7.7 LMH, salt rejection of 97.9 %, and reverse solute flux of 0.506 gMH at low flow rates in the FO desalination process.

Keywords: desalination, forward osmosis, membrane performance, polyethyleneimine, polyethylene glycol, reduced graphene oxide, stability

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Authors: Arifa Batool, Ghulam Hussain Bhatti, Syed Mujtaba Shah

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Inorganic n-type (TiO2, CdO) and p-type (NiO, CuO) metal oxide nanoparticles were synthesized by a facile wet chemical method at room temperature. The morphological, compositional, structural and optical properties were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, FT-IR, XRD analysis, UV/Visible and fluorescence spectroscopy. All semiconducting nanoparticles were photosensitized with Ru (II) based Z907 dye in ethanol solvent by grafting. Grafting of dye on the surface of nanoparticles was confirmed by UV/Visible and FT-IR spectroscopy. The synthesized photo-active nanohybrid was thoroughly blended with P3HT, a solid electrolyte and I-V measurements under solar stimulated radiations 1000 W/m2 (AM 1.5) were recorded. Maximum incident photon to current conversion efficiency (IPCE) of 0.9% was achieved with dye functionalized Z907-TiO2 hybrid, IPCE of 0.72% was achieved with bulk-heterojunction of TiO2-Z907-CuO and IPCE of 0.68% was attained with nanocomposite of TiO2-CdO. TiO2 based Solar cells have maximum Jscvalue i.e.4.63 mA/cm2. Dye-functionalized TiO2-based photovoltaic devices were found more efficient than the reference device but the morphology of the device was a major check in progress.

Keywords: solar cell, bulk heterojunction, nanocomposites, photosensitization, dye sensitized solar cell

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Authors: Saima Nasreen, Uzaira Rafique, Shery Ehrman, Muhammad Aqeel Ashraf

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The release of heavy metals into the environment is a potential threat to water and soil quality as well as to plant, animal and human health. In current research work, organically functionalized mesoporous silicates (MSU-H) were prepared by the co-condensation between sodium silicate and oregano alkoxysilanes in the presence of the nonionic surfactant triblock copolymer P104. The surfactant was used as a template for improving the porosity of the hybrid gels. Synthesized materials were characterized by TEM, FT-IR, SEM/EDX, TG, surface area analysis. The surface morphology and textural properties of such materials varied with various kinds of groups in the channels. In this study, removal of some heavy metals ions from aqueous solution by adsorption process was investigated. Batch adsorption studies show that the adsorption capacity of metal ions on the functionalized silicates is more than that on pure MSU-H. Data shows adsorption on synthesized materials is a time efficient process, suggesting adsorption on external surface as well as the mesoporous process. Adsorption models of Langmuir, Freundlich, and Temkin depicted equal goodness for all adsorbents, whereas pseudo 2nd order kinetics is in best agreement with experimental data.

Keywords: heavy metals, mesoporous silica, hybrid, adsorption, freundlich, langmuir, temkin

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Authors: Xinyu Wei, Mingming Peng, Kenji Kamiya, Eika Qian

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Iso-stearic acid as a saturated fatty acid with a branched chain shows a low pour point, high oxidative stability and great biodegradability. The industrial production of iso-stearic acid involves first isomerizing unsaturated fatty acids into branched-chain unsaturated fatty acids (BUFAs), followed by hydrogenating the branched-chain unsaturated fatty acids to obtain iso-stearic acid. However, the production yield of iso-stearic acid is reportedly less than 30%. In recent decades, extensive research has been conducted on branched fatty acids. Most research has replaced acidic clays with zeolites due to their high selectivity, good thermal stability, and renewability. It was reported that isomerization of unsaturated fatty acid occurred mainly inside the zeolite channel. In contrast, the production of by-products like dimer acid mainly occurs at acid sites outside the surface of zeolite. Further, the deactivation of catalysts is attributed to the pore blockage of zeolite. In the present study, micro/mesoporous ZSM-22 zeolites were developed. It is clear that the synthesis of a micro/mesoporous ZSM-22 zeolite is regarded as the ideal strategy owing to its ability to minimize coke formation. Different mesoporosities micro/mesoporous H-ZSM-22 zeolites were prepared through recrystallization of ZSM-22 using sodium hydroxide solution (0.2-1M) with cetyltrimethylammonium bromide template (CTAB). The structure, morphology, porosity, acidity, and isomerization performance of the prepared catalysts were characterized and evaluated. The dissolution and recrystallization process of the H-ZSM-22 microporous zeolite led to the formation of approximately 4 nm-sized mesoporous channels on the outer surface of the microporous zeolite, resulting in a micro/mesoporous material. This process increased the weak Brønsted acid sites at the pore mouth while reducing the total number of acid sites in ZSM-22. Finally, an activity test was conducted using oleic acid as a model compound in a fixed-bed reactor. The activity test results revealed that micro/mesoporous H-ZSM-22 zeolites exhibited a high isomerization activity, reaching >70% selectivity and >50% yield of BUFAs. Furthermore, the yield of oligomers was limited to less than 20%. This demonstrates that the presence of mesopores in ZSM-22 enhances contact between the feedstock and the active sites within the catalyst, thereby increasing catalyst activity. Additionally, a portion of the dissolved and recrystallized silica adhered to the catalyst's surface, covering the surface-active sites, which reduced the formation of oligomers. This study offers distinct insights into the production of iso-stearic acid using a fixed-bed reactor, paving the way for future research in this area.

Keywords: Iso-stearic acid, oleic acid, skeletal isomerization, micro/mesoporous, ZSM-22

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Authors: Qiong Tian, Lifeng Zhang, Demei Yu, Ajit D. Kelkar

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Low specific weight and high strength is the basic requirement for aerospace materials. Fiber-reinforced epoxy resin composites are attractive materials for this purpose. Boron nitride nanoparticles (BNNPs) have good radiation shielding capacity, which is very important to aerospace materials. Herein a processing route for an advanced hybrid composite material is demonstrated by introducing dispersed BNNPs in standard prepreg manufacturing. The hybrid materials contain three parts: E-fiberglass, an aerospace-grade epoxy resin system, and BNNPs. A vacuum assisted resin transfer molding (VARTM) was utilized in this processing. Two BNNP functionalization approaches are presented in this study: (a) covalent functionalization with 3-aminopropyltriethoxysilane (KH-550); (b) non-covalent functionalization with cetyltrimethylammonium bromide (CTAB). The functionalized BNNPs were characterized by Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction(XRD) and scanning electron microscope (SEM). The results showed that BN powder was successfully functionalized via the covalent and non-covalent approaches without any crystal structure change and big agglomerate particles were broken into platelet-like nanoparticles (BNNPs) after functionalization. Compared to pristine BN powder, surface modified BNNPs could result in significant improvement in mechanical properties such as tensile, flexural and compressive strength and modulus. CTAB functionalized BNNPs (CTAB-BNNPs) showed higher tensile and flexural strength but lower compressive strength than KH-550 functionalized BNNPs (KH550-BNNPs). These reinforcements are mainly attributed to good BNNPs dispersion and interfacial adhesion between epoxy matrix and BNNPs. This study reveals the potential in improving mechanical properties of BNNPs-containing composites laminates through surface functionalization of BNNPs.

Keywords: boron nitride, epoxy, functionalization, prepreg, composite

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