Search Results (232)

In this study, a novel, highly efficient, environment friendly, and low-cost nanocatalyst, denoted as Ni(x)@Co−N−C, was successfully developed by encapsulating Ni nanoparticles into N-doped porous carbon derived from ZIF-67. A variety of techniques including powder X-ray diffraction (XRD), nitrogen adsorption/desorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectrometer (XPS) were used to characterize the prepared materials. The TEM images reveal that the nanoparticles were distributed homogeneously in the carbon support. The N atoms in the carbon support serve as the sites for the nucleation and uniform growth of Ni nanoparticles. The catalyst was used for the degradation of environmentally harmful 4-nitrophenol (4-NP) to 4-aminophenol (4-AP). Among all the catalysts investigated, Ni(10)@Co-N-C exhibited the highest catalytic activity for the hydrogenation of 4-NP, with a specific reaction rate of 6.1 × 10⁻³ s⁻¹, activity parameter of 31 s⁻¹g⁻¹, and turn over frequency (TOF) of 1.78 × 10¹⁹ molecules g_metal⁻¹s⁻¹. On the other hand, the specific reaction rate and TOF value were 1.7 × 10⁻³ s⁻¹ and 6.96 × 10¹⁸ molecules g_metal⁻¹s⁻¹, respectively, for Co−N−C. This suggests that Ni(10)@Co−N−C is about three times more catalytically active than the Co−N−C catalyst. The superb activity of Ni(10)@Co−N−C in comparison to Co−N−C can be ascribed to the homogeneous dispersion of small-sized Ni nanoparticles, the interconnected three-dimensional porous arrangement of the support Co−N−C, the presence of N atoms in the carbon framework that stabilize metal nanoparticles, and the synergistic electronic effect between Ni and Co. The Ni(10)@Co−N−C catalyst maintained consistent catalytic activity over multiple cycles, which suggests that porous N-containing carbon support can effectively prevent aggregation and leaching of metal nanoparticles. The ICP-AES analysis of the recycled Ni(10)@Co−N−C revealed a slight reduction in metal content compared to the fresh sample, suggesting almost negligible leaching of metal nanoparticles. Full article

We report a method for the synthesis of 2-substituted benzoxazoles from tertiary amides and 2-aminophenols in the presence of triflic anhydride (Tf₂O) and 2-Fluoropyridine (2-F-Pyr). The cascade reaction involves the activation of the amide carbonyl group by Tf₂O, nucleophilic addition, intramolecular cyclization, and elimination. Furthermore, we explore the scope of this method by varying both the amide and 2-aminophenol substrates, highlighting its versatility in the synthesis of a wide range of functionalized benzoxazole derivatives. Full article

Background/Objectives: The most used antipyretic and pain relief treatment is paracetamol (acetaminophen), also known as N-acetyl-para-aminophenol (APAP). However, it is considered potentially hazardous if consumed repeatedly in large doses or over prolonged periods. This investigation explores the effectiveness of hesperidin (Hesp) and Hesp loaded on layered double hydroxide nanoparticles (Hesp-NPs) in inhibiting the progression of acute hepatotoxicity in rats induced by APAP. Methods: LDH-Hesp-NPs were prepared and characterized. Male Wistar rats were orally treated with Hesp and Hesp-NPs at the same adjusted dose (100 mg/kg) every other day for six weeks. After 2 h of the first doses of Hesp and Hesp-NPs, the rats received one oral dose of APAP (750 mg/kg). Results: Administering of Hesp and Hesp-NPs to APAP-treated rats significantly reduced oxidant parameter (malondialdehyde) and serum enzymes (ALT, AST, LDH, and ALP) associated with liver function. Antioxidant markers in the liver, such as catalase and glutathione, also increased notably. Moreover, Hesp and Hesp-NPs enhanced the mRNA expression of liver UGT1A6, IL-10, and HO-1. Conversely, the mRNA expressions of liver CYP1A1, KEAP1, TGF-β, P53, and BAX decreased. These improvements in biochemical and molecular markers were corroborated by liver histopathology. Conclusions: Hesp and Hesp-NPs protect significantly against APAP-induced hepatotoxicity in male Wistar rats. Hesp-NPs treatment was more potent. The protective effects may be mediated via modulation of APAP biotransformation, oxidative stress, inflammation and apoptosis. Full article

The availability of water-soluble nanoparticles allows catalytic reactions to occur in highly desirable green environments. The catalytic activity and selectivity of water-soluble palladium nanoparticles capped with 6-(carboxylate)hexanethiolate (C6-PdNP) and 5-(trimethylammonio)pentanethiolate (C5-PdNP) were investigated for the reduction of 4-nitrophenol, the oxidation of α,β-conjugated aldehydes, and the C-C coupling of phenylboronic acid. The study showed that between the two PdNPs, C6-PdNP exhibits better catalytic activity for the reduction of 4-nitrophenol to 4-aminophenol in the presence of sodium borohydride and the selective oxidation of conjugated aldehydes to conjugated carboxylic acids. For the latter reaction, molecular hydrogen (H₂) and H₂O act as oxidants for the surface palladium atoms on PdNPs and conjugated aldehyde substrates, respectively. The results indicated that the competing addition activities of Pd-H and H₂O toward the π-bond of different unsaturated substrates promote either reduction or oxidation reactions under mild conditions in organic solvent-free environments. In comparison, C5-PdNP exhibited higher catalytic activity for the C-C coupling of phenylboronic acid. Gas chromatography–mass spectrometry (GC-MS) was mainly used as an analytical technique to examine the products of catalytic reactions. Full article

In this study, three dinuclear copper(II) complexes of ligand 2,6-bis[(N-methyl-piperazine-1-yl)methyl]-4-formyl phenol (L1) and one of 2,6-bis[(N-methylpiperazine-1-yl)methyl]-4-formyl phenol dimethylacetal (L2) with copper(II) ions have been investigated as new types of biomimetic catalysts for the oxidative transformation of different aminophenols and phenyldiamines. All the complexes of interest were newly synthesized and further characterized by IR spectroscopy, UV-Vis and mass spectrometry, X-ray diffraction, and selected electrochemical measurements. Crystal structures of these dinuclear copper(II) complexes have revealed that the coordination-shell geometry of copper atoms is close to a tetragonal pyramid. Catecholase, phenoxazinone synthase, and horseradish peroxidase-like activities were observed in pure methanol and water–methanol mixtures in the presence of molecular oxygen. The potential applicability of the complexes under study is discussed with respect to their possibilities and limitations in the replacement of natural copper-containing oxidoreductases in the oxidative degradation of water-insoluble chlorinated aminophenols in the dye industry or in the production of phenoxazine-based drugs. Full article

The reduction of unfriendly 4-nitrophenol to make it unimpactful with the environment (4-aminophenol) was carried out using the metastable form of copper ferrite (CuFe₅O₈) synthesized by the co-precipitation of metal nitrate salts, an efficient method with inexpensive and abundant starting materials. The samples were obtained by calcination at various temperatures ranging from 600 °C to 900 °C. The material characterizations, including X-ray diffraction, N₂ adsorption/desorption, scanning electron microscope, X-ray absorption spectroscopy, and ultraviolet–visible spectrometry, were employed to identify the detailed structures and describe their correlations with catalytic activities. The X-ray diffraction and X-ray absorption spectroscopy analyses revealed the presence of mixed CuFe₅O₈ and copper oxide phases, where the formers are rich in Cu²⁺, Fe²⁺, and Fe³⁺ ions. The electron transfer between Cu²⁺, Fe²⁺, and Fe³⁺ led to the high efficiency of the catalytic reaction of the synthesized copper ferrites. Especially for the sample calcined at 600 °C, the apparent kinetic constant (k) for a reduction of 4-nitrophenol was equal to 0.25 min⁻¹, illustrating nearly 100% conversion of 4-nitrophenol to 4-aminophenol within less than 9 min. Regarding the N₂ adsorption/desorption isotherms, the samples calcined at 600 °C have the highest specific Brunauer–Emmett–Teller (BET) surface area (15.93 m² g⁻¹) among the others in the series, which may imply the most effective catalytic performance investigated herein. The post-catalytic X-ray diffraction investigation indicated the stability of the prepared catalysts. Furthermore, the chemical stability of the prepared catalysts was confirmed by its reusability in five consecutive cycles. Full article

Emerging pollutants, such as N-acetyl-para-aminophenol, pose significant challenges to environmental sustainability, and Bi₂Fe₂O₂ (BFO) nanomaterials are an emerging class of piezoelectric materials. This study presents a novel piezoelectric-driven Fenton system based on Bi₂Fe₄O₉ nanosheets for the efficient degradation of organic pollutants. BFO nanosheets with varying thicknesses were synthesized, and their piezoelectric properties were confirmed through piezoresponse force microscopy and heavy metal ion reduction experiments. The piezoelectric electrons generated within the BFO nanosheets facilitate the in situ production of hydrogen peroxide, which in turn drives the Fenton-like reaction. Furthermore, the piezoelectric electrons enhance the redox cycling of iron in the Fenton process, boosting the overall catalytic efficiency. The energy band structure of BFO nanosheets is well-suited for this process, enabling efficient hydrogen peroxide generation and promoting Fe³⁺ reduction. The findings demonstrate that thinner BFO nanosheets exhibit superior piezoelectric activity, leading to enhanced catalytic performance. Additionally, the incorporation of gold nanodots onto BFO nanosheets further boosts their piezocatalytic efficiency, particularly in the reduction of Cr (VI). The system exhibited robust oxidative capacity, stability, and recyclability, with reactive oxygen species (ROS) verified via electron paramagnetic resonance spectroscopy. Overall, BFO nanosheets, with their optimal energy band structure, self-supplied hydrogen peroxide, and enhanced Fe³⁺ reduction, represent a promising, sustainable solution for advanced oxidation processes in wastewater treatment and other applications. Full article

New aromatic co-polyamide-imides (coPAIs) containing both carboxyl and hydroxyl groups in the repeating units were synthesized for the first time. Transport, thermal and morphological properties of dense nonporous membranes from PAIs obtained using the diacid chloride of 2-(4-carboxyphenyl)-1,3-dioxoisoindoline-5-carboxylic acid and diamines 5,5′-methylene-bis (2-aminophenol)) and 3,5-Diaminobenzoic acid, taken in molar ratios of 7:3, 1:1, and 3:7, have been studied. High levels of membrane permeability accompanied by high selectivity for mixtures of liquids with significantly different polarities were determined by realization of intra- and intermolecular interactions in polymer, which was proved by thermal analyses and hydrodynamic characteristics of coPAIs. This effect is discussed in the context of the effectiveness of intermolecular interactions between polymer chains containing carboxyl and hydroxyl functional groups. Full article

The determination of formaldehyde is of paramount importance, as it is present in numerous locations throughout life. In this study, aminophenol-modified gold nanoparticles (ATP-AuNPs) with different relative positions of hydroxyl and amino groups were synthesized for the detection of formaldehyde. They were characterized by transmission electron microscopy (TEM), ultraviolet–visible (UV-Vis) spectroscopy and Fourier transform infrared (FTIR) spectroscopy tests. The results demonstrated that the position plays a crucial role in the composites, which exhibit good stability when the sulfhydryl group and amino group transition from the para position to the neighboring position. Furthermore, the para position was identified as the optimal configuration for formaldehyde detection. When it was used to detect formaldehyde in ultrapure and Li River water, the limit of detection (LOD) was calculated to be 1.03/1.15 mM, respectively. This work not only provides a novel ATP-AuNP sensor but also highlights its practical situations. Full article

A series of new quinazolin-2,4-dione derivatives incorporating amide/eight-membered nitrogen-heterocycles 2a–c, in addition, acylthiourea/amide/dithiolan-4-one and/or phenylthiazolidin-4-one 3a–d and 4a–d. The starting compound 1 was prepared by reaction of 4-(2,4-dioxo-1,4-dihydro-2H-quinazolin-3-yl)-benzoyl chloride with ammonium thiocyanate and cyanoacetic acid hydrazide. The reaction of 1 with strong electrophiles, namely, o-aminophenol, o-amino thiophenol, and/or o-phenylene diamine, resulted in corresponding quinazolin-2,4-dione derivatives incorporating eight-membered nitrogen-heterocycles 2a–d. Compounds 3a–d and 4a–d were synthesized in good-to-excellent yield through a one-pot multi-component reaction (MCR) of 1 with carbon disulfide and/or phenyl isocyanate under mild alkaline conditions, followed by ethyl chloroacetate, ethyl iodide, methyl iodide, and/or concentrated HCl, respectively. The obtained products were physicochemically characterized by melting points, elemental analysis, and spectroscopic techniques, such as FT-IR, ¹H-NMR, ¹³C-NMR, and MS. The antibacterial efficacy of the obtained eleven molecules was examined in vitro against two Gram-positive bacterial strains (Staphylococcus aureus and Staphylococcus haemolyticus). Furthermore, Computer-Aided Drug Design (CADD) was performed on the synthesized derivatives, standard drug (Methotrexate), and reported antibacterial drug with the target enzymes of bacterial strains (S. aureus and S. haemolyticus) to explain their binding mode of actions. Notably, our findings highlight compounds 2b and 2c as showing both the best antibacterial activity and docking scores against the targets. Finally, according to ADMET predictions, compounds 2b and 2c possessed acceptable pharmacokinetics properties and drug-likeness properties. Full article

Yearly, thousands of tons of wasted coffee grounds are produced according to high coffee consumption. Still, after the coffee brewing, wasted coffee grounds contain some amounts of caffeine (CAF). CAF, in turn, contains multiple O and N chelating atoms in its structure. These have a potential to be reductors for complexes of metals. In this context, within the present study, a set of CAF extracts derived from coffee beans and coffee grounds were obtained and then used for the one-step reduction of ReO₄⁻ ions with no additional toxic chemicals. Within this approach, CAF was applied as a secondary, green resource for the synthesis of unique rhenium nanoparticles (ReNPs) containing Re species at 0 and +6 oxidation states. The obtained ReNPs were identified and characterized with the use of X-ray powder diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM). Further, the capping and stabilization of ReNPs by CAF were verified with the aid of Fourier transformation infrared spectroscopy (FT-IR). The so-obtained “green” ReNPs were then used as a homogenous catalyst in the catalytic hydrogenation of 4-nitrophenol (4-NP). This new nanomaterial revealed a superior catalytic activity, leading to the complete reduction of 4-NP to 4-aminophenol within 40–60 min with a first-order rate constant of 0.255 min⁻¹. Full article

This study investigates the significant impact of metal–support interactions on catalytic reaction mechanisms at the interface of oxide-supported metal nanoparticles. The distinct and contrasting effects of SiO₂ and TiO₂ supports on reaction dynamics using NaBD₄ were studied and focused on the relative yields of [HD]/[H₂] and [D₂]/[H₂]. The findings show a consistent increase in HD yields with rising [BD₄⁻] concentrations. Notably, the sequence of HD yield enhancement follows the order of TiO₂-Au⁰-NPs < Au⁰-NPs < SiO₂-Au⁰-NPs. Conversely, the rate of H₂ evolution during BH₄^- hydrolysis exhibits an inverse trend, with TiO₂-Au⁰-NPs outperforming the others, followed by Au⁰-NPs and SiO₂-Au⁰-NPs, demonstrating the opposing effects exerted by the TiO₂ and SiO₂ supports on the catalytic processes. Further, the catalytic reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) confirms the catalytic mechanism, with TiO₂-Au⁰-NPs demonstrating superior activity. The catalytic activity observed aligns with the order of TiO₂-Au⁰-NPs > Au⁰-NPs > SiO₂-Au⁰-NPs, suggesting that SiO₂ donates electrons to Au⁰-NPs, while TiO₂ withdraws them. It is of interest to note that two very different processes, that clearly proceed via different mechanisms, are affected similarly by the supports. This study reveals that the choice of support material influences catalytic activity, impacting overall yield and efficiency. These findings underscore the importance of selecting appropriate support materials for tailored catalytic outcomes. Full article

With the utilization of nitrophenols in manufacturing various materials and the expansion of industry, nitrophenols have emerged as water pollutants that pose significant risks to both humans and the environment. Therefore, it is imperative to convert nitrophenols into aminophenols, which are less toxic. This conversion process is achieved through the use of noble metal nanoparticles, such as gold, silver, copper, and palladium. The primary challenge with noble metal nanoparticles lies in their accumulation and deactivation, leading to a decrease in catalyst activity. Covalent organic frameworks (COFs) are materials characterized by a crystalline structure, good stability, and high porosity with active sites. These properties make them ideal substrates for noble metal nanoparticles, enhancing catalytic activity. This overview explores various articles that focus on the synthesis of catalysts containing noble metal nanoparticles attached to COFs as substrates to reduce nitrophenols to aminophenols. Full article

The compound p-Nitrophenol (p-NP) is widely recognized as a highly toxic nitro-aromatic substance that urgently requires emission control. Reducing p-NP to p-aminophenol (p-AP) not only decreases its toxicity and mineralization properties in nature but also provides a key raw material for the chemical and pharmaceutical industries. The study used coal fly ash (CFA) as a catalyst carrier for synthesizing the p-NP reduction catalyst. Using CFA as an alternative option not only reduces costs but also achieves the objective of treating waste with waste compared to utilizing commercial solid materials for synthesizing catalysts. By employing hydrochloric acid and sodium hydroxide pretreatment methods, the physicochemical properties of CFA are significantly improved, enhancing the dispersion of palladium (Pd) nanoparticles. The structural features of the prepared samples were characterized using various surface analysis techniques, and both intermittent and continuous modes were experimentally tested for the model catalytic reaction involving the sodium borohydride (NaBH₄)-mediated reduction of p-NP. The results demonstrate that CFA has potential in wastewater treatment. Full article

Catalytic performance decline is a general issue when shaping fine powder into macroscale catalysts (e.g., beads, fiber, pellets). To address this challenge, a phenolic resin-assisted strategy was proposed to prepare porous Co/N carbon beads (ZACBs) at millimeter scale via the phase inversion method followed by confined pyrolysis. Specially, p-aminophenol–formaldehyde (AF) resin-coated zeolitic imidazolate framework (ZIF-67) nanoparticles were introduced to polyacrylonitrile (PAN) solution before pyrolysis. The thermosetting of the coated AF improved the interface compatibility between the ZIF-67 and PAN matrix, inhibiting the shrinkage of ZIF-67 particles, thus significantly improving the void structure of ZIF-67 and the dispersion of active species. The obtained ZACBs exhibited a 99.9% removal rate of tetracycline (TC) within 120 min, with a rate constant of 0.069 min⁻¹ (2.3 times of ZIF-67/PAN carbon beads). The quenching experiments and electron paramagnetic resonance (EPR) tests showed that radicals dominated the reaction. This work provides new insight into the fabrication of high-performance MOF catalysts with outstanding recycling properties, which may promote the use of MOF powder in more practical applications. Full article