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Due to the rapid technological advancements of various sectors in recent decades, there has been a growing need for energy, necessitating the development of large-capacity, robust, adaptable, and economical energy storage systems. The most current energy-storage material known as “MXene” is a two-dimensional layered transition metal nitride or carbonitride and carbide. A covalently bonded layer is exfoliated from its parent MAX (Mn + 1AXn) phase by selective chemical etching. MXene commands the highest demand of all the two-dimensional families of materials due to its extraordinary characteristics, which include high conductivity, flexible surface functional groups, excellent mechanical properties, superior hydrophilicity, electrochemical nature, and the thickness of its atomic layers. MXene is used in solid-state supercapacitors, batteries, antimicrobial films, gas and biosensors, water splitting, electromagnetic interference shielding, and photo- and electrocatalysis. Because of MXene’s special qualities, researchers are concentrating on developing the material further, both theoretically and experimentally. Utilizing a variety of microfabrication processes, MXene microelectrodes of micro-sized energy storage devices (MESDs) have been previously created. Distinct methodologies influence not only the apparatus’s arrangement but also the composition of MXene microelectrodes and the electrochemical efficacy of MESDs. ,This review study addresses relevant topics and provides a topical summary of the state-of-the-art regarding MXene-based energy storage devices. The field’s challenges and prospects for the future are discussed in the final part.

Among various clear energy generation processes, electrocatalytic water splitting or hydrogen evolution reaction (HER) has been considered as an efficient method for the sustainable production of hydrogen (H2) fuel. But, significant efforts are still required to develop cheap, effective and stable electrocatalysts for water splitting to achieve the economical production of H2. In the quest of finding cheap electrocatalysts, herein, we demonstrate the preparation of palladium (Pd) nanoparticles decorated nitrogen (N) doped highly reduced graphene oxide (NDG-Pd) based electrocatalysts. The nitrogen (N) doped highly reduced graphene oxide (NDG) was produced by using graphene oxide as precursor, which was reduced and doped with nitrogen, simultaneously in one-step hydrothermal method. Subsequently, Pd nanoparticles were decorated on the surface of NDG using a facile ultrasonic method to produce NDG-Pd. In order to restrict the amount of precious metal to reduce the cost of catalysts, very small percentage of Pd, such as, 1 and 3 % was utilized during the preparation of electrocatalysts. The as-prepared electrocatalysts were successfully characterized by using different methods such as, XRD, XPS, EDX, BET, SEM and TEM. Results confirmed the formation of slightly agglomerated, smaller size of Pd NPs on the surface of NDG with an average particle size of ∼ 6 nm. The as prepared nanocomposites NDG, NDG-Pd1% and NDG-Pd3% were used to prepare electrodes and their electrocatalytic activity was evaluated towards the production of H2 through water splitting. The results of electrochemical performance of as-prepared electrodes within the voltage range have revealed that among different samples prepared, the NDG did not show any current, whereas NDG-Pd3% showed a good potential for HER with current density ≈24 mA/cm2 at very low potential i.e. −0.2 V vs RHE.

A superabsorbent polymer, Sodium Alginate-g-Poly (Itaconic acid-co-Sodium 4-vinyl benzenesulfonate)/ Ricinus communis (SA-g-P(ITA-co-VBS)/ RC) hydrogel, was prepared by free-radical graft co-polymerization for sequestration of toxic malachite green (MG) dye as a cationic dye model. The surface morphological of shape and composition of the prepared hydrogel used have been characterized by FESEM, EDX, TEM, FTIR, X-ray diffraction XRD, and TGA. Optimizing the synthesis conditions for prepared a hydrogel with the highest swelling ratio have been studied, the results show that employing 0.08 g KPS and 0.09 g MBA, 1.0 g ITA, 2.0 g VBS, 1.0 g SA, and 1.0 g RC, the composites greatest swelling capacity in distilled water was 3400 %. It was discovered that the dye adsorption capacity of the polymer was greatly impacted by the monomer VBS level in the hydrogel, which gives it a better ability to swell. The porosity of the hydrogel spheres, thus significantly enhancing the MG adsorption capacity with the rate-limiting controlled by chemical adsorption, intraparticle diffusion, and film diffusion. Study the influence of different reaction conditions on the removal of MG dye from aqueous solution are adsorbent dose, pH, zero-point charge, temperature, thermodynamic adsorption, adsorption isotherm, and kinetic models have been done. Additionally, (SA-g-P(ITA-co-VBS)/RC) demonstrated strong MG dye adsorption capabilities and reusability in at least four adsorption-desorption cycles this process indicating its considerable potential for use as the adsorbent for dye removals from aqueous solution.

Palladium (Pd), a noble metal, has unique properties for C-C bond formation in reactions such as the Suzuki and Heck reactions. Besides Pd-based complexes, Pd NPs have also attracted significant attention for applications such as fuel cells, hydrogen storage, and sensors for gases such as H2 and non-enzymatic glucose, including catalysis. Additionally, Pd NPs are catalysts in environmental treatment to abstract organic and heavy-metal pollutants such as Cr (VI) by converting them to Cr(III). In terms of biological activity, Pd NPs were found to be active against Staphylococcus aureus and Escherichia coli, where 99.99% of bacteria were destroyed, while PVP-Pd NPs displayed anticancer activity against human breast cancer MCF7. Hence, in this review, we attempted to cover recent progress in the various applications of Pd NPs with emphasis on their application as sensors and catalysts for energy-related and other applications.

The utilization of heterogeneous catalysts during the production of biodiesel potentially minimize the cost of processing due to the exclusion of the separation step. The (X wt%)Ni–ZrO2 (where X = 10, 25 and 50) catalysts prepared through a hydrothermal process were tested for the production of biodiesel by the transesterification of waste cooking oil (WCO) with methanol. The influences of various reaction parameters were systematically optimized. While the physicochemical characteristics of the as-synthesized catalysts were examined using numerous techniques such as FTIR, XRD, TGA BET, EDX, SEM, and HRTEM. Among all the catalysts, (10 wt%)Ni–ZrO2 exhibited high surface area when compared to the pristine ZrO2, (25 wt%)Ni–ZrO2 and (50 wt%)Ni–ZrO2 nanocatalysts. It may have influenced the catalytic properties of (10 wt%)Ni–ZrO2, which exhibited maximum catalytic activity with a biodiesel production yield of 90.5% under optimal conditions. Such as 15:1 methanol to oil molar ratio, 10 wt% catalysts to oil ratio, 8 h reaction time and 180 °C reaction temperature. Furthermore, the recovered catalyst was efficiently reused in several repeated experiments, demonstrating marginal loss in its activity after multiple cycles (five times).

Application of nanoparticles in drug delivery has become an emerging phenomenon. This is typically achieved either via custom made nanoparticles or through the functionalization of pre-synthesized nanoparticles with the pharmaceutically active ingredients. In this study, Pregabalin, which is the active pharmaceutical ingredient of commercially available drug Lyrica, is used to functionalize pre-synthesized gold nanoparticles (AuNPs). The work was divided into two parts. The first part determined by synthesis of AuNPs. The second part was achieving conjugation of the AuNPs with Pregabalin to obtain nanocomposites (AuNPs-PGN). AuNPs formed were nanosized, spherical in shape, with a particle size ~35 nm. The probable nanocomposite formation takes place by conjugation between AuNPs and the carboxyl group (COOH) of Pregabalin.

Cellulose is a polysaccharide composed of D-glucopyranose linked by 1,4 β-glycoside bond with three hydroxyl groups. These hydroxyl groups in cellulose have an important role in the compactness of crystalline structure and in determining the physical properties of cellulose. Cellulose in nanometers size range from 10 nm to 350 nm is known as nano cellulose, which has a variety of applications due to the unique properties such as low density, biodegradable, and good mechanical properties. In the present study, we present the isolation of the nano cellulose from flaxseed hull for the first time. The isolated nano cellulose was characterized by techniques such as UV–Vis, FT-IR, BET, XRD SEM, and TEM. The nano cellulose obtained was found to be crystalline in nature with a crystallinity index of 46% and the surface area of 5 cm2/g with excellent thermal stability. Keywords: Nanocrystals, Cellulose, Flaxseeds, XRD, FTIR, SEM

This work reports the synthesis of nickel/nickel hydroxides nanoflakes (Ni/Ni(OH)2-NFs) at room temperature via a novel chemical deposition and exfoliation from a liquid crystal template mixture. The nickel ions dissolved in the interstitial aqueous domain of the Brij®78 hexagonal liquid crystal template were deposited by a reducing agent of sodium borohydride that concurrently reduces the nickel ions and generates extreme hydrogen gas bubbles, that exfoliated the nickel/nickel hydroxide layers. The Ni/Ni(OH)2-NFs crystal structure, morphology, and surface area characterizations revealed the formation of semi-crystalline α-Ni(OH)2 nanoflakes with a thickness of approximately 10 nm and a specific surface area of about 135 m2/g. The electrochemical measurements of cyclic voltammetry, chronoamperometry, and impedance analysis showed that the Ni/Ni(OH)2-NFs exhibited significant performance for the glucose non-enzymatic oxidation in an alkaline solution in comparison to the bare-nickel hydroxide (bare-Ni(OH)2) deposited without surfactant. The Ni/Ni(OH)2-NFs electrode showed superior glucose oxidation activity over the bare-Ni(OH)2 catalyst with a sensitivity of 1.078 mA mM−1 cm−2 with a linear concentration dependency range from 0.2 to 60 mM and a detection limit of 0.2 mM (S/N = 3). The enhanced electrochemical active surface area and mesoporosity of the 2D nanoflakes make the Ni/Ni(OH)2-NFs a promising catalyst in the application of glucose non-enzymatic sensing.

This work demonstrates hydrazine electro-oxidation and sensing using an ultrathin copper oxide nanosheet (CuO-NS) architecture prepared via a versatile foam-surfactant dual template (FSDT) approach. CuO-NS was synthesised by chemical deposition of the hexagonal surfactant Brij®58 liquid crystal template containing dissolved copper ions using hydrogen foam that was concurrently generated by a sodium borohydride reducing agent. The physical characterisations of the CuO-NS showed the formation of a two-dimensional (2D) ultrathin nanosheet architecture of crystalline CuO with a specific surface area of ~39 m2/g. The electrochemical CuO-NS oxidation and sensing performance for hydrazine oxidation revealed that the CuO nanosheets had a superior oxidation performance compared with bare-CuO, and the reported state-of-the-art catalysts had a high hydrazine sensitivity of 1.47 mA/cm2 mM, a low detection limit of 15 μM (S/N = 3), and a linear concentration range of up to 45 mM. Moreover, CuO-NS shows considerable potential for the practical use of hydrazine detection in tap and bottled water samples with a good recovery achieved. Furthermore, the foam-surfactant dual template (FSDT) one-pot synthesis approach could be used to produce a wide range of nanomaterials with various compositions and nanoarchitectures at ambient conditions for boosting the electrochemical catalytic reactions.

Nanoparticles (NPs) prepared through safer, eco-friendly and natural-based products can be used various applications including antimicrobial and biomedical applications. Quorum sensing (QS) is a complex system for intercellular communication that regulates the expression of many virulence determinants, in the opportunistic Pseudomonas aeruginosa. Thus, the disruption of QS-mediated communication system could be an alternative strategy to combat infection caused by drug resistant P. aeruginosa. In this study, zinc oxide nanoparticles (ZnO NPs) were synthesized by using seed extract of Butea monosperma and further characterized by XRD, SEM and TEM. The biosynthesized ZnO NPs were then subjected to the investigation of their antibacterial, antibiofilm activities as well as the anti-quorum sensing potentialities for biomedical applications. The minimum inhibitory concentration (MIC) value against P. aeruginosa was found 1600 µg/ml, and it was found that ZnO NPs effectively reduced virulence factors Viz. swarming and swimming of P. aeruginosa by 62.8 and 45%, respectively. Exopolysaccharides production was also affected by ZnO NPs which indicate the disruption of biofilm formation. Further, the in silico docking analysis displayed that ZnO NPs efficiently interacted within QS (Las/Rhl) mechanism of P. aeruginosa by binding to the catalytic cleft of LasI synthase (Gly-116-ZnO = 2.8 Å), RhlI synthase (Gly-180-ZnO = 3.7 Å) and transcription receptor protein LasR receptor (Asn-141-ZnO = 2.9 Å), RhlR receptor (Tyr-72-ZnO = 2.6 Å). Thus, it was concluded that the effective interaction of ZnO NPs with Las and Rhl system led to the inactivation of autoinducers such as N-acyl homoserine lactones (AHL) molecules which finally led to the inactivation of QS and down regulation of virulence determinants. Consequently, the present in vitro and in silico results obtained suggest that the synthesized ZnO NPs can be efficiently used as potent antimicrobial agents to prevent the colonization, biofilm formation as well as anti-QS-mediated determinants caused by pathogenic drug resistant bacteria.

The use of heterogeneous catalyst for biodiesel production can reduce the price of separation process and therefore minimize the biodiesel cost. ZnCuO/N-doped graphene (NDG) catalyst synthesized by facile mechanochemical procedure was tested in the transesterification of waste cooking oil (WCO) with methanol to produce biodiesel. The effects of catalyst loading (0–15 wt%), weight percentage of NDG (10–100%), methanol to oil molar ratio (6:1–18:1), reaction time (2–10 h) and reaction temperature (120–200 °C) were systematically studied at the optimal conditions. Additionally, the properties of the fabricated catalysts were assessed via XRD, FTIR, N2 sorption studies, HRTEM, TGA and Raman spectroscopy. It was found that the ZnCuO/(X%)NDG nanocomposites exhibit enhanced catalytic performance when compared with the ZnCuO catalyst (without NDG) under the identical conditions. The efficacy of the ZnCuO/(X%)NDG nanocomposites has improved owing to the inclusion of NDG in the catalytic system, which in-turn enhanced the properties of the mixed metal oxides (MMO’s) such as surface area, defective sites to a great extent. The ZnCuO/(30%)NDG catalyst displayed a highest catalytic activity towards transesterification of WCO (97.1%) at the optimized conditions of 10 wt% catalyst loading, 15:1 methanol:oil molar ratio, 8 h reaction time and 180 °C reaction temperature. Moreover, the recovered catalyst was successfully reused six cycles with no discernible loss in its activity.

Catalytic efficacy of metal-based catalysts can be significantly enhanced by doping graphene or its derivatives in the catalytic protocol. In continuation of previous work regarding the catalytic properties of highly-reduced graphene oxide (HRG), graphene-oxide (GO) doped mixed metal oxide-based nanocomposites, herein we report a simple, straightforward and solventless mechanochemical preparation of N-doped graphene (NDG)/mixed metal oxide-based nanocomposites of ZnO–MnCO3 (i.e., ZnO–MnCO3/(X%-NDG)), wherein N-doped graphene (NDG) is employed as a dopant. The nanocomposites were prepared by physical milling of separately fabricated NDG and ZnO–MnCO3 calcined at 300 °C through eco-friendly ball mill procedure. The as-obtained samples were characterized via X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), Raman, Field emission scanning electron microscopy (FESEM), Energy-dispersive X-ray spectroscopy (EDX) and surface area analysis techniques. To explore the effectiveness of the obtained materials, liquid-phase dehydrogenation of benzyl alcohol (BOH) to benzaldehyde (BH) was chosen as a benchmark reaction using eco-friendly oxidant (O2) without adding any harmful surfactants or additives. During the systematic investigation of reaction, it was revealed that the ZnO–MnCO3/NDG catalyst exhibited very distinct specific-activity (80 mmol/h.g) with a 100% BOH conversion and 3). Under the optimum catalytic conditions, the catalyst successfully transformed various aromatic, heterocyclic, allylic, primary, secondary and aliphatic alcohols to their respective ketones and aldehydes with high selectively and convertibility without over-oxidation to acids. In addition, the ZnO–MnCO3/NDG was also recycled up to six times with no apparent loss in its efficacy.

Green and eco-friendly synthesis of palladium nanoparticles NPs is carried out under facile and eco-friendly conditions using an aqueous solution of Salvadora persica L. (SP) root extract (RE) as a bioreductant, which is commonly known as Miswak. The as-synthesized Pd NPs were characterized using various spectroscopic and microscopic techniques, including, UV–Vis spectroscopy, FT-IR spectroscopy, XRD, ICP-MS and TEM. Detailed investigations of the Pd NPs have confirmed that the polyphenolic phytomolecules present in the RE of Miswak not only act as a bioreductant by facilitating the reduction and growth of Pd NPs, but they also functionalize the surface of Pd NPs and stabilized them in various solvents. Furthermore, the catalytic activity of the green synthesized Pd NPs was also tested toward the Suzuki coupling reactions of various aryl halides in aqueous media. The as-prepared Pd NPs exhibited superior catalytic activity and reusability for the Suzuki coupling reaction in aqueous and aerobic conditions. The kinetics of the reaction studied by GC revealed that the conversion of various aryl halides to biphenyl takes place in a short time.

Due to their excellent physicochemical properties and synergistic effect, graphene metallic NPs based nanocomposites have gained significant attention in various technological fields including catalysis. Here we demonstrate a single pot, facile and environmental friendly synthesis of catalytically active palladium(Pd)@graphene nanocomposites (SP-HRG-Pd) by the simultaneous reduction of graphene oxide (GRO) and PdCl2 using Salvadora persica L. (miswak) root extract (RE) as bioreductant. The synthesis of SP-HRG-Pd was confirmed by various spectroscopic and microscopic techniques, including ultraviolet–visible (UV–vis), Fourier-transform infrared (FT-IR), Raman and X-ray photoelectron (XPS) spectroscopy, X-ray powder diffraction (XRD) and transmission electron microscopy (TEM). The polyphenolic (flavonoids) and terpenoids rich contents of the miswak RE not only facilitated the reduction of graphene oxide and PdCl2 but also ensured the homogeneous binding of the Pd NPs on graphene, and through stabilization of the surface of SP-HRG-Pd nanocomposites. This also led to the enhanced dispersibility of as synthesized nanocomposites in aqueous solutions. The as-prepared SP-HRG-Pd nanocomposites also demonstrated excellent catalytic activity toward the selective oxidation of aromatic alcohols. Furthermore, in order to study the effect of calcination temperature and concentration of Pd NPs on the catalytic activities of nanocomposites, different samples of SP-HRG-Pd nanocomposites containing different amounts of Pd using various concentrations of Pd precursor were prepared and calcined at various temperatures.

In recent years, the development of green mechanochemical processes for the synthesis of new catalysts with higher catalytic efficacy and selectivity has received manifest interest. In continuation of our previous study, in which graphene oxide (GRO) and highly reduced graphene oxide (HRG) based nanocomposites were prepared and assessed, herein, we have explored a facile and solvent-less mechanochemical approach for the synthesis of N-doped graphene (NDG)/mixed metal oxide (MnCO3–ZrO2) ((X%)NDG/MnCO3–ZrO2), as the (X%)NDG/MnCO3–ZrO2 nano-composite was synthesized using physical grinding of separately synthesized NDG and pre-calcined (300 °C) MnCO3–ZrO2 via green milling method. The structures of the prepared materials were characterized in detail using X-ray powder diffraction (XRD), Field Emission Scanning Electron Microscope (FESEM), Energy Dispersive X-Ray Analysis (EDX), Fourier-transform infrared spectroscopy (FTIR), Raman, Thermogravimetric analysis (TGA), and N2 adsorption-desorption isotherm analysis. Besides, the obtained nanocomposites were employed as heterogeneous oxidation catalyst for the alcohol oxidation using green oxidant O2 without involving any surfactants or bases. The reaction factors were systematically studied during the oxidation of benzyl alcohol (PhCH2OH) as the model reactant to benzaldehyde (PhCHO). The NDG/MnCO3–ZrO2 exhibits premium specific activity (66.7 mmol·g−1·h−1) with 100% conversion of PhCH2OH and > 99.9% selectivity to PhCHO after only 6 min. The mechanochemically prepared NDG based nanocomposite exhibited notable improvement in the catalytic efficacy as well as the surface area compared to the pristine MnCO3–ZrO2. Under the optimal circumstances, the NDG/MnCO3–ZrO2 catalyst could selectively catalyze the aerobic oxidation of a broad array of alcohols to carbonyls with full convertibility without over-oxidized side products like acids. The NDG/MnCO3–ZrO2 catalyst were efficiently reused for six subsequent recycling reactions with a marginal decline in performance and selectivity.

Plant extract of Pulicaria undulata (L.) was used as both reducing agent and stabilizing ligand for the rapid and green synthesis of gold (Au), silver (Ag), and gold–silver (Au–Ag) bimetallic (phase segregated/alloy) nanoparticles (NPs). These nanoparticles with different morphologies were prepared in two hours by stirring corresponding metal precursors in the aqueous solution of the plant extracts at ambient temperature. To infer the role of concentration of plant extract on the composition and morphology of NPs, we designed two different sets of experiments, namely (i) low concentration (LC) and (ii) high concentration (HC) of plant extract. In the case of using low concentration of the plant extract, irregular shaped Au, Ag, or phase segregated Au–Ag bimetallic NPs were obtained, whereas the use of higher concentrations of the plant extract resulted in the formation of spherical Au, Ag, and Au–Ag alloy NPs. The as-prepared Au, Ag, and Au–Ag bimetallic NPs showed morphology and composition dependent catalytic activity for the reduction of 4-nitrophenol (4-NPh) to 4-aminophenol (4-APh) in the presence of NaBH4. The bimetallic Au–Ag alloy NPs showed the highest catalytic activity compared to all other NPs.

Recently, the development of eco-friendly mechanochemical approaches for the preparation of novel catalysts with enhanced activity and selectivity has gained considerable attention. Herein, we developed a rapid and solvent-less mechanochemical method for the preparation of mixed metal oxide (Ag2O−MnO2) decorated graphene oxide (GRO)-based nanocomposites (Ag2O−MnO2/(X wt.%)GRO), as the Ag2O−MnO2/(X wt.%)GRO nanocomposite was fabricated by the physical grinding of freshly prepared GRO and pre-annealed (300 °C) mixed metal oxide nanoparticles (NPs) (Ag2O−MnO2) using an eco-friendly milling procedure. The as-prepared nanocatalysts were characterized by using various techniques. Furthermore, the nanocomposites were applied as a heterogeneous catalyst for the oxidation of alcohol by employing gaseous O2 as an eco-friendly oxidant under base-free conditions. The mechanochemically obtained GRO-based composite exhibited noticeable enhancement in the surface area and catalytic performance compared to the pristine Ag2O−MnO2. The results revealed that (1%)Ag2O−MnO2/(5 wt.%)GRO catalyst exhibited higher specific performance (13.3 mmol·g−1·h−1) with a 100% conversion of benzyl alcohol (BnOH) and >99% selectivity towards benzaldehyde (BnH) within 30 min. The enhancement of the activity and selectivity of GRO-based nanocatalyst was attributed to the presence of various oxygen-containing functional groups, a large number of defects, and a high specific surface area of GRO. In addition, the as-prepared nanocatalyst also demonstrated excellent catalytic activity towards the conversion of a variety of other alcohols to respective carbonyls under optimal conditions. Besides, the catalyst ((1%)Ag2O−MnO2/(5 wt.%)GRO) could be efficiently recycled six times with no noticeable loss in its performance and selectivity.

The catalytic activity of copper-manganese (CuMn2) mixed oxide nanoparticles (Cu/Mn = 1:2) has been studied for the selective oxidation of benzylic alcohols to the corresponding aldehydes using molecular oxygen as an oxidizing agent. The CuMn2 mixed oxide showed excellent catalytic activity for the oxidation of benzylic alcohols to the corresponding aldehydes with high selectivity (>99%). The complete conversion (100%) of all the benzylic alcohols to the corresponding aldehydes is achieved within a short reaction period at 102 °C. The catalytic performance is obtained to be dependent on the electronic and steric effects of the substituents present on the phenyl ring. Electron withdrawing and bulky groups attached to the phenyl ring required longer reaction time for a complete conversion of the benzylic alcohols.

A green, one-step approach for the preparation of graphene/Ag nanocomposites (PE-HRG-Ag) via simultaneous reduction of both graphene oxide (GRO) and silver ions using Pulicaria glutinosa plant extract (PE) as reducing agent is reported. The plant extract functionalizes the surfaces of highly reduced graphene oxide (HRG) which helps in conjugating the Ag NPs to HRG. Increasing amounts of Ag precursor enhanced the density of Ag nanoparticles (NPs) on HRG. The preparation of PE-HRG-Ag nanocomposite is monitored by using ultraviolet–visible (UV-Vis) spectroscopy, powder X-ray diffraction (XRD), and energy dispersive X-ray (EDX). The as-prepared PE-HRG-Ag nanocomposities display excellent surface-enhanced Raman scattering (SERS) activity, and significantly increased the intensities of the Raman signal of graphene.

Zinc oxide nanoparticles doped manganese carbonate catalysts [X% ZnOx–MnCO3] (where X = 0–7) were prepared via a facile and straightforward coprecipitation procedure, which upon different calcination treatments yields different manganese oxides, that is, [X% ZnOx–MnO2] and [X% ZnOx–Mn2O3]. A comparative catalytic study was conducted to evaluate the catalytic efficiency between carbonates and oxides for the selective oxidation of secondary alcohols to corresponding ketones using molecular oxygen as a green oxidizing agent without using any additives or bases. The prepared catalysts were characterized by different techniques such as SEM, EDX, XRD, TEM, TGA, BET, and FTIR spectroscopy. The 1% ZnOx–MnCO3 calcined at 300°C exhibited the best catalytic performance and possessed highest surface area, suggesting that the calcination temperature and surface area play a significant role in the alcohol oxidation. The 1% ZnOx–MnCO3 catalyst exhibited superior catalytic performance and selectivity in the aerial oxidation of 1-phenylethanol, where 100% alcohol conversion and more than 99% product selectivity were obtained in only 5 min with superior specific activity (48 mmol·g−1·h−1) and 390.6 turnover frequency (TOF). The specific activity obtained is the highest so far (to the best of our knowledge) compared to the catalysts already reported in the literatures used for the oxidation of 1-phenylethanol. It was found that ZnOx nanoparticles play an essential role in enhancing the catalytic efficiency for the selective oxidation of alcohols. The scope of the oxidation process is extended to different types of alcohols. A variety of primary, benzylic, aliphatic, allylic, and heteroaromatic alcohols were selectively oxidized into their corresponding carbonyls with 100% convertibility without overoxidation to the carboxylic acids under base-free conditions.

This work reports the zirconia (ZrOx) nanoparticles doped MnCO3 catalysts prepared by facile and simple coprecipitation technique and the synthesis of zirconia-manganese carbonate [X% ZrOx–MnCO3] (where X% = 0–7%) catalyst which upon calcination at 400°C is converted to zirconia-manganese dioxide [1% ZrOx–MnO2] and when calcined at 500°C is converted to zirconia-manganic trioxide [1% ZrOx–Mn2O3]. A comparative catalytic study was performed to investigate the catalytic efficiency between carbonate and oxides for the selective oxidation of 1-phenylethanol by using molecular O2 as a clean oxidant. The influence of several parameters such as w/w% of ZrOx, reaction time, calcination temperature, catalyst amount, and reaction temperature has been thoroughly examined using oxidation of 1-phenylethanol as a model substrate. The 1% ZrOx–MnCO3 precalcined at 300°C exhibited the best catalytic efficiency. It was found that ZrOx nanoparticles also play an essential role in enhancing the effectiveness of the catalytic system for the aerobic oxidation of alcohols. Furthermore, the physical and chemical properties of synthesized catalysts were evaluated by microscopic and spectroscopic techniques. An extremely high specific activity of 40 mmol·g−1·h−1 with a 100% conversion of oxidation product and selectivity of >99% was achieved within extremely short reaction time (6 min).

Graphene and its nanocomposites are showing excellent potential in improving the catalytic performances of different materials. However, the synthetic protocol and its form, such as graphene oxide (GRO) or highly reduced graphene oxide (HRG), influence the catalytic efficiencies. Here, we present, a facile synthesis of graphene oxide (GRO) and ZrOx-MnCO3-based nanocomposites [(1%)ZrOx−MnCO3/(x%)GRO] and their outcome as an oxidation catalyst for alcohol oxidation under mild conditions using O2 as a clean oxidant. The ZrOx−MnCO3/GRO catalyst prepared by incorporating GRO to pre-calcined ZrOx-MnCO3 using ball milling showed remarkable enhancement in the catalytic activities as compared to pristine ZrOx−MnCO3, ZrOx−MnCO3 supported on HRG or ZrOx−MnCO3/GRO prepared by in-situ growth of ZrOx−MnCO3 onto GRO followed by calcination. The catalyst with composition (1%)ZrOx−MnCO3/(1%)GRO exhibited superior specific activity (57.1 mmol/g·h) with complete conversion and >99% selectivity of the product within a short period of time (7 min) and at a relatively lower temperature (100 °C). The catalyst could be recycled at least five times with a negligible decrease in efficiency and selectivity. The catalytic study was extended to different aromatic as well as aliphatic alcohols under optimized conditions, which confirmed the efficiency and selectivity of the catalyst.

Nitrogen-doped graphene (NDG)-palladium (Pd)-based nanocatalysts (NDG@Pd) can be potentially applied as an efficient catalyst for the preparation of biaryls in a Suzuki−Miyaura coupling reaction. Herein, we report the one-pot facile synthesis of an NDG@Pd nanocatalyst, wherein the nanocatalyst was prepared by the simultaneous reduction of graphene oxide (GRO) and PdCl2 in the presence of hydrazine hydrate as a reducing agent, while ammonium hydroxide was used as a source of “N’’ on the surface of graphene. The as-synthesized NDG@Pd nanocatalyst, consisting of smaller-sized, spherical-shaped palladium nanoparticles (Pd-NPs) on the surface of NDG, was characterized by several spectroscopic and microscopic techniques, including high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), ultraviolet−visible spectroscopy (UV-Vis), Fourier-transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and Brunauer−Emmett−Teller (BET). The nanocatalyst displayed outstanding catalytic activity in the Suzuki−Miyaura cross-coupling reactions of phenyl halides with phenyl boronic acids under facile conditions in water. The catalytic activity of NDG@Pd was found to be a more efficient catalyst when compared to pristine highly reduced graphene oxide (HRG) based Pd nanocatalyst (HRG@Pd). Furthermore, the reusability of the catalyst was also tested by repeatedly performing the same reaction using the recovered catalyst. The N-doped catalyst displayed excellent reusability even after several reactions.

A single-step solvothermal approach to prepare stabilized cubic zirconia (ZrO2) nanoparticles (NPs) and highly reduced graphene oxide (HRG) and ZrO2 nanocomposite (HRG@ZrO2) using benzyl alcohol as a solvent and stabilizing ligand is presented. The as-prepared ZrO2 NPs and the HRG@ZrO2 nanocomposite were characterized using transmission electron microscopy (TEM) and X-ray diffraction (XRD), which confirmed the formation of ultra-small, cubic phase ZrO2 NPs with particle sizes of ~2 nm in both reactions. Slight variation of reaction conditions, including temperature and amount of benzyl alcohol, significantly affected the size of resulting NPs. The presence of benzyl alcohol as a stabilizing agent on the surface of ZrO2 NPs was confirmed using various techniques such as ultraviolet-visible (UV-vis), Fourier-transform infrared (FT-IR), Raman and XPS spectroscopies and thermogravimetric analysis (TGA). Furthermore, a comparative electrochemical study of both as-prepared ZrO2 NPs and the HRG@ZrO2 nanocomposites is reported. The HRG@ZrO2 nanocomposite confirms electronic interactions between ZrO2 and HRG when compared their electrochemical studies with pure ZrO2 and HRG using cyclic voltammetry (CV).

Ag2O nanoparticles-doped MnO2 decorated on different percentages of highly reduced graphene oxide (HRG) nanocomposites, i.e., (X%)HRG/MnO2–(1%)Ag2O (where X = 0–7), were fabricated through straight-forward precipitation procedure, and 400 °C calcination, while upon calcination at 300 °C and 500 °C temperatures, it yielded MnCO3 and manganic trioxide (Mn2O3) composites, i.e., [(X%)HRG/MnCO3–(1%)Ag2O] and [(X%)HRG/Mn2O3–(1%)Ag2O], respectively. These nanocomposites have been found to be efficient and very effective heterogeneous catalysts for selective oxidation of secondary alcohols into their respective ketones using O2 as a sole oxidant without adding surfactants or nitrogenous bases. Moreover, a comparative catalytic study was carried out to investigate the catalytic efficiency of the synthesized nanocomposites for the aerobic oxidation of 1-phenylethanol to acetophenone as a substrate reaction. Effects of several factors were systematically studied. The as-prepared nanocomposites were characterized by TGA, XRD, SEM, EDX, HRTEM, BET, Raman, and FTIR. The catalyst with structure (5%)HRG/MnO2–(1%)Ag2O showed outstanding specific activity (16.0 mmol/g·h) with complete conversion of 1-phenylethanol and >99% acetophenone selectivity within short period (25 min). It is found that the effectiveness of the catalyst has been greatly improved after using graphene support. A broad range of alcohols have selectively transformed to desired products with 100% convertibility and no over-oxidation products have been detected. The recycling test of (5%)HRG/MnO2–(1%)Ag2O catalyst for oxidation of 1-phenylethanol suggested no obvious decrease in its performance and selectivity even after five subsequent runs.

Nanocomposites of highly reduced graphene oxide (HRG) and ZnOx nanoparticles doped manganese carbonate containing different percentages of HRG were prepared via a facile co-precipitation method. The prepared sample calcined at 300 °C yielded i.e., ZnOx(1%)–MnCO3/(X%)HRG (where X = 0–7), calcination at 400 °C and 500 °C, yielded different manganese oxides i.e., ZnOx(1%)–MnO2/(X%)HRG and ZnOx(1%)–Mn2O3/(X%)HRG respectively. The prepared catalyst were subjected to catalytic evaluation and a comparative catalytic study between carbonates and oxides for the liquid-phase aerobic oxidation of benzylic alcohols to corresponding aldehydes using molecular oxygen as an eco-friendly oxidant without adding additives or bases. The influence of various parameters such as percentage of HRG, reaction time, catalyst amount, calcination and reaction temperature was systematically examined to optimize reaction conditions using oxidation of benzyl alcohol as a substrate model. It was found that the catalytic performance is remarkably enhanced after using HRG as catalyst co-dopant for the aerobic oxidation of alcohols, possibly owing to the presence of carbon defects and oxygenated functional groups on HRG surface. The as-synthesized catalysts were characterized by SEM, EDX, XRD, Raman, TGA, BET, and FT-IR. Under optimal conditions, the catalyst with composition ZnOx(1%)–MnCO3/(1%)HRG calcined at 300 °C exhibited remarkable specific activity (57.1 mmol·g−1·h−1) with 100% conversion of benzyl alcohol and more than 99% product selectivity within extremely short time (7 min). The as-prepared catalyst was re-used up to five consecutive times without significant decrease in its activity and selectivity. To the best of our knowledge, the achieved specific activity is the highest so far compared to the earlier reported catalysts used for the benzyl alcohol oxidation. A wide range of substituted benzylic and aliphatic alcohols were selectively oxidized into their corresponding aldehydes with complete convertibility and selectivity in short reaction times without over-oxidation to the acids. Due to their significant low cost, superior reproducibility, excellent catalytic efficiency, the ZnOx(1%)–MnCO3/(X%)HRG nanocomposites possess several application prospect in other organic chemistry reactions.

The synthesis of Palladium (Pd) nanoparticles by green methods has attracted remarkable attention in recent years because of its superiority above chemical approaches, owing to its low cost and ecological compatibility. In this present work, we describe a facile and environmentally friendly synthesis of Pd nanoparticles (Pd NPs) using an aqueous extract of aerial parts of Origanum vulgare L. (OV) as a bioreductant. This plant is available in many parts of the world as well as in Saudi Arabia and is known to be a rich source of phenolic components, a feature we fruitfully utilized in the synthesis of Pd NPs, using various concentrations of plant extracts. Moreover, the OV extract phytomolecules are not only accountable for the reduction and progression of nanoparticles, but they also act as stabilizing agents, which was confirmed by several characterization methods. The as-synthesized Pd nanoparticles (Pd NPs) were analyzed using ultraviolet-visible spectroscopy (UV-Vis), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), and thermal gravimetric analysis (TGA). Further, FT-IR study has proven that the OV not merely represents a bioreductant but also functionalizes the nanoparticles. Furthermore, the green synthesized metallic Pd NPs were successfully applied as catalysts for selective oxidation of alcohols.

Suzuki-Miyaura coupling reaction catalyzed by the palladium (Pd)-based nanomaterials is one of the most versatile methods for the preparation of biaryls. However, use of organic solvents as reaction medium causes a big threat to environment due to the generation of toxic byproducts as waste during the work up of these reactions. Therefore, the use of water as reaction media has attracted tremendous attention due to its environmental, economic, and safety benefits. In this study, we report on the synthesis of green Pd@graphene nanocatalyst based on an in situ functionalization approach which exhibited excellent catalytic activity towards the Suzuki–Miyaura cross-coupling reactions of phenyl halides with phenyl boronic acids under facile conditions in water. The green and environmentally friendly synthesis of Pd@graphene nanocatalyst (PG-HRG-Pd) is carried out by simultaneous reduction of graphene oxide (GRO) and PdCl2 using Pulicaria glutinosa extract (PGE) as reducing and stabilizing agent. The phytomolecules present in the plant extract (PE) not only facilitated the reduction of PdCl2, but also helped to stabilize the surface of PG-HRG-Pd nanocatalyst, which significantly enhanced the dispersibility of nanocatalyst in water. The identification of PG-HRG-Pd was established by various spectroscopic and microscopic techniques, including, high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), ultraviolet–visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FT-IR), and Raman spectroscopy. The as-prepared PG-HRG-Pd nanocatalyst demonstrated excellent catalytic activity towards the Suzuki-Miyaura cross coupling reactions under aqueous, ligand free, and aerobic conditions. Apart from this the reusability of the catalyst was also evaluated and the catalyst yielded excellent results upon reuse for several times with marginal loss of its catalytic performance. Therefore, the method developed for the green synthesis of PG-HRG-Pd nanocatalyst and the eco-friendly protocol used for the Suzuki coupling offers a mild and effective substitute to the existing protocols and may significantly contribute to the endeavors of green chemistry.

Catalytic activity of copper-manganese mixed oxide nanoparticles (Cu/Mn = 1 : 2) prepared by coprecipitation method has been studied for selective oxidation of benzyl alcohol using molecular oxygen as an oxidizing agent. The copper-manganese (CuMn2) oxide catalyst exhibited high specific activity of 15.04 mmolg−1 h−1 in oxidation of benzyl alcohol in toluene as solvent. A 100% conversion of the benzyl alcohol was achieved with >99% selectivity to benzaldehyde within a short reaction period at 102°C. It was found that the catalytic performance is dependent on calcination temperature, and best activity was obtained for the catalyst calcined at 300°C. The high catalytic performance of the catalyst can be attributed to the formation of active MnO2 phase or absence of less active Mn2O3 phase in the mixed CuMn2 oxide. The catalyst has been characterized by powder X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer Emmett-Teller (BET) surface area measurement, and Fourier transform infrared (FT-IR) spectroscopies.

Microbicidal potential of silver nanoparticles (Ag-NPs) can be drastically improved by improving their solubility or wettability in the aqueous medium. In the present study, we report the synthesis of both green and chemical synthesis of Ag-NPs, and evaluate the effect of the dispersion qualities of as-prepared Ag-NPs from both methods on their antimicrobial activities. The green synthesis of Ag-NPs is carried out by using an aqueous solution of readily available Salvadora persica L. root extract (RE) as a bioreductant. The formation of highly crystalline Ag-NPs was established by various analytical and microscopic techniques. The rich phenolic contents of S. persica L. RE (Miswak) not only promoted the reduction and formation of NPs but they also facilitated the stabilization of the Ag-NPs, which was established by Fourier transform infrared spectroscopy (FT-IR) analysis. Furthermore, the influence of the volume of the RE on the size and the dispersion qualities of the NPs was also evaluated. It was revealed that with increasing the volume of RE the size of the NPs was deteriorated, whereas at lower concentrations of RE smaller size and less aggregated NPs were obtained. During this study, the antimicrobial activities of both chemically and green synthesized Ag-NPs, along with the aqueous RE of S. persica L., were evaluated against various microorganisms. It was observed that the green synthesized Ag-NPs exhibit comparable or slightly higher antibacterial activities than the chemically obtained Ag-NPs.

Polyacrylic acid (PAA) is an important industrial chemical, which has been extensively applied in various fields, including for several biomedical purposes. In this study, we report the synthesis and modification of this polymer with various phenol imides, such as succinimide, phthalimide and 1,8-naphthalimide. The as-synthesized derivatives were used to prepare polymer metal composites by the reaction with Zn+2. These composites were characterized by using various techniques, including NMR, FT-IR, TGA, SEM and DSC. The as-prepared PAA-based composites were further evaluated for their anti-microbial properties against various pathogens, which include both Gram-positive and Gram-negative bacteria and different fungal strains. The synthesized composites have displayed considerable biocidal properties, ranging from mild to moderate activities against different strains tested.