One-pot Hydrothermal Synthesis Research Articles

Effective fenton catalyst from controllable framework doping of Fe in porous silica spheres

Controllable doping of iron (Fe) (3.9–17.8%) in hollow porous silica spheres with highly homogeneous distribution state was achieved successfully by a one-pot hydrothermal synthesis strategy. Based on the observation and analysis by transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, nitrogen sorption, and X-ray photoelectron spectroscopy (XPS), it was found that molecular Fe species were intercalated into silica framework during the structural transformation of silica to hollow flake-shelled spheres, which leads to both stable fixation with open accessibility of Fe and high surface area of the Fe-doped silica hollow spheres (Fe-SHSs). When used as heterogeneous Fenton catalyst to degrade the dye of Acid orange 7 (AO7), enhanced catalysis performance was exhibited due to the sufficiently exposed active sites and fast mass transport in the system. The optimal catalysis condition was also studied by adjusting Fe-SHSs dosages, oxidant concentrations, and pH values). This work presents an effective strategy for chemical doping of metal components in the silica structures and may also be explored for other supported metal catalyst systems.

One-Pot Hydrothermal Synthesis of Functionalized Mesoporous Silica for Effective Removal of Pb(II) Ion

There is a huge scope for the removal of heavy metal ions from aqueous solutions. In this study, mesoporous silica materials, (MSMs), functionalized with (3-Mercaptopropyl) trimethoxysilane, (MPTS/MSMs), were prepared and used for adsorption of Pb(II) ions from aqueous solutions. The synthesis of MPTS/MSMs adsorbent was done using one-pot hydrothermal method by immobilizing 3-Mercaptopropyl trimethoxysilane onto mesoporous silica surface. The structure and properties of the adsorbent were explored using different techniques such as FT-IR, XRD, SEM, TEM, TGA, and N2 adsorption-desorption isotherms. The adsorption applicability of prepared nanostructure for removal of the Pb(II) ions from the aqueous solution was investigated and the results showed a good selectivity in the absorption of Pb(II) ions over other ions in aqueous solution. The effect of different parameters including the solution pH, Pb(II) concentration, sorbent amount, ion interfering effect, and the contact time onto the removal efficiency of the adsorbent was investigated systematically. The maximum adsorption efficiency (~ 97%) was found for the solutions with pH = 6, the best contact time was seen as 30 min for 50 mg L−1 of the analyte under the optimal conditions. The adsorbent was triumphantly used for the removal of Pb (II) ions from the three real water samples, including tap water, well water, and lake water with the removal efficiency of > 95%.

Fine-tuning the surface acidity of hierarchical zeolite composites for methanol-to-olefins (MTO) reaction

The zeolite nanosheet composites, containing a high acidic density ZSM-5 and weak-acidic Silicalite-1 nanosheets (Si-NS) acting as a core and a shell, respectively, have been successfully fabricated by a one-pot hydrothermal synthesis. The shell thickness, textural properties, and acidity of synthesized composites can be easily adjusted by hydrothermal synthesis time and temperature. The uniform thickness of 9.4 ± 1.1 nm of Silicalite-1 shells can be observed when using the crystallization temperature of 110 °C, whereas the non-uniform distribution of zeolite shells becomes predominant with increasing the crystallization temperature due to its rapid growing rate. Interestingly, due to the different acidity of core and shell materials, the acid site distribution of the composites has been modified with respect to their isolated zeolites, and therefore the highly selective production of propylene in MTO process is greatly improved (>90% and 50% for the hierarchical composite and unmodified ZSM-5, respectively). In addition, a significantly lower coke formation could be achieved due to the suppression of further side reactions over the stacking-layered siliceous covering on high acidic density ZSM-5 surfaces. This example opens up perspectives for the development of hierarchical zeolite composites with the modified acid surfaces for highly selective production of light olefins.

One-Pot Hydrothermal Synthesis of La-Doped ZnIn2S4 Microspheres with Improved Visible-Light Photocatalytic Performance.

Impurity element doping is extensively taken as one of the most efficient strategies to regulate the electronic structure as well as the rate of photogenerated charge separation of photocatalysts. Herein, a one-pot hydrothermal synthesis process was exploited to obtain La-doped ZnIn2S4 microspheres, aiming at gaining insight into the role that doping ions played in the improvement of pollutant photodegradation. Systematical characterization means, comprising of X–ray photoelectron spectroscopy (XPS), ultraviolet–visible (UV–vis) diffuse reflection spectroscopy and Raman spectra, combination with high-resolution transmission electron microscopy (HRTEM), were employed to in depth reveal the concomitancy of La ions and ZnIn2S4 crystal lattice. The results showed that the La-doped ZnIn2S4 samples exhibited a slightly wider and stronger spectral absorption than pristine ZnIn2S4; and the specific surface area of doped ZnIn2S4 samples was a bit larger. The La-doped ZnIn2S4 electrodes showed improved photocurrent response, and the photocurrent density reached a maximum value at La content of 1.5 wt%. As expected, La-doped ZnIn2S4 samples exhibited a remarkable enhancement of photocatalytic behaviour toward the photodegradation of tetracycline hydrochloride (TCH) and methyl orange (MO). The prominently enhanced photoactivity of doped ZnIn2S4 samples was due to the synergistic effect of the elevated visible-light absorption ability and effective photogenerated charge carriers’ separation.

One-pot hydrothermal synthesis of dual metal incorporated CuCe-SAPO-34 zeolite for enhancing ammonia selective catalytic reduction

A series of dual metal incorporated CuCex-SAPO-34(x = 0–0.04) samples were synthesized using one-pot hydrothermal method with diethylamine as organic structure-directing agent for selective catalytic reduction of NOx by NH3. The catalytic properties were elucidated in detail with physicochemical properties being analyzed using various instruments. All the catalysts exhibited typical SAPO-34 crystal structures with high specific surface areas. With the dual-metal incorporation, the surface acidity and amount of isolated Cu2+, which may be active sites for NH3-SCR, were significantly enhanced. However, excessive Ce restrained the formation of isolated Cu2+ due to its occupation of cationic sites. Therefore, the 0.05CuCe0.02-SAPO-34 exhibited high NO conversion (≥80%) at 168°C-500°C. Furthermore, the NH3-SCR mechanism over different catalysts was investigated in-situ DRIFTS experiments. For the 0.05Cu-SAPO-34, the adsorbed NH3 species react with gaseous NO and following the E-R mechanism throughout the reaction temperature range. Meanwhile, adsorbed NO2 was detected and reacted with the adsorbed NH3 species according to the L-H mechanism in low-temperature region. In contrast, the NH3-SCR reaction over the 0.05CuCe0.02-SAPO-34 primarily followed the E-R mechanism throughout the temperature range. The L-H mechanism was cut off due to the loss of the adsorption ability of nitrous species at high temperatures., resulting in NO conversion decreasing.

One-pot synthesis of hierarchical CdS/MoS2/rGO with enhanced (photo)electrocatalytic activities

A facile one-pot hydrothermal synthesis of 3D windmill-like CdS/MoS2/rGO has been reported. The MoS2/rGO framework prevents the aggregation of CdS and leads to a two-pathway for electron transfer, thus enhancing the electron density and more active site on the rGO surface. Compared with pure CdS, the hierarchical CdS/MoS2/rGO catalyst displays superior photocatalytic H2 production activity and electrocatalytic H2 evolution overpotential, which is 3.5 times in photoactivity and 146.7 mV decrease of overpotential. A new hierarchical structure and its characteristics and mechanism are proposed at the atomic-/nanoscale.

One-Pot Hydrothermal Synthesis of MoS2/Zn0.5Cd0.5S Heterojunction for Enhanced Photocatalytic H2 Production.

A series of molybdenum disulfide (MoS2)/Zn0.5Cd0.5S heterojunctions have been prepared via a mild one-pot hydrothermal method based on the optimization of composition content of primary photocatalyst. The photocatalysts demonstrated significantly improved visible light–driven photocatalytic activity toward H2 evolution from water without using any noble metal cocatalyst. Among the as-prepared composites, 0.2% MoS2/Zn0.5Cd0.5S shows the best performance. The highest H2 evolution rate reaches 21 mmol · g−1 · h−1, which is four times higher than that of pure Zn0.5Cd0.5S. The apparent quantum efficiency is about 46.3% at 425 nm. The superiority is attributed to the tight connection between MoS2 and Zn0.5Cd0.5S by this facile one-step hydrothermal synthesis. As a result, the formation of the heterostructure introduces built-in electric field at the interface that facilitates vectorial charge transfer. More specifically, photogenerated electrons transfer to MoS2 to conduct proton reduction, where the holes are retained on the surface of Zn0.5Cd0.5S to react with the sacrificial reagents. Moreover, the composite presents improved stability without notable activity decay after several cycled tests.

One-pot hydrothermal synthesis of a magnetic hydroxyapatite nanocomposite for MR imaging and pH-Sensitive drug delivery applications

Synthetic hydroxyapatite (HA) due to its high biocompatibility, anti-inflammatory properties, high stability, and a flexible structure in combination with magnetic nanoparticles has the strong potential to be used in modern medicine including tissue engineering, imaging, and drug delivery. Herein, a hydrothermal process was used to prepare magnetite nanoparticles dispersed on the hydroxyapatite nanorods with cetyltrimethylammonium bromide (CTAB) as a surfactant. Characterization study of the synthesized iron oxide-hydroxyapatite (IO-HA) nanocomposite was performed by FT-IR spectroscopy, X-ray powder diffraction, energy dispersive X-Ray analysis (EDX) for elemental mapping, transmission electron microscopy, and vibrating sample magnetometer. Then, the biocompatibility of the synthesized nanocomposite studied by 3-(4,5-dimethylthiazol-2-yl) -2,5-diphenyltetrazolium bromide (MTT) assay and hemocompatibility assay. Focus on this point, curcumin loaded IO-HA (Cur@IO-HA) was developed for exploring the pH-sensitivity of the drug carrier and then evaluating its cellular uptake. The in vitro efficacy of the synthesized nanocomposites as a magnetic resonance imaging (MRI) contrast agent was also investigated. Our results showed that IO-HA nanocomposite is non-cytotoxic and hemocompatible as well as a good pH-sensitive drug carrier and a favorable MRI T2 contrast agent. Comparing to the free curcumin, Cur@IO-HA displayed a good cellular uptake. Taking into account the above issues, IO-HA nanocomposite has the most potential for application as a theranostic MRI contrast agent.

One-pot hydrothermal synthesis of dual Z-scheme BiOBr/g-C3N4/Bi2WO6 and photocatalytic degradation of tetracycline under visible light

Bi2WO6/g-C3N4/BiOBr composite was simply synthesized by a one-pot hydrothermal process and exhibited excellent photocatalytic activities in Tetracycline degradation under visible light for 40 min with high efficiency of 90% due to the obviously increased charge separation. Photoelectrochemical measurements and radical (OH, h+ and O2−) trapping experiments deduced the electron transfer mechanism. This work provided a facile synthesis method for bismuth based ternary heterostructures with potential applications in environmental remediation.

Cost-effective single-step synthesis of flower-like cerium-ruthenium-sulfide for the determination of antipsychotic drug trifluoperazine in human urine samples

Nanostructured binary metal sulfides are considered as a promising electrode material because of their excellent electron transfer and good sensing behavior rather than metal oxides. As a result, the binary metal sulfides were applied in energy and electrochemical sensor applications. Herein, we propose the electrochemical sensor method based on flower-like cerium-ruthenium sulfide nanostructure (Ce–Ru–S NS) for the electrochemical sensing of trifluoperazine (TFPZ). The Ce–Ru–S NS prepared using the cost-effective one-pot hydrothermal synthesis technique. Then, the resultant materials were characterized through suitable spectrophotometric techniques and the electrocatalytic properties of the fabricated sensor were investigated by EIS, CV, and amperometric (i–t) techniques. The Ce–Ru–S material has good electrocatalytic activity towards the electrochemical oxidation of TFPZ. Significantly, the fabricated sensor demonstrates the distinct amperometric response with the lowest limit of detection (LOD) of 0.322 nM (S/N = 3), high sensitivity 2.682 μA μM−1 cm−2 and lowest oxidation potential of +0.64 V (Ag/AgCl). Furthermore, the Ce–Ru–S NS displays excellent selectivity, good reproducibility, and long-term stability. The practicability of the TFPZ sensor tested in a human urine sample.

Boosting the cyclic stability and supercapacitive performance of graphene hydrogels via excessive nitrogen doping: Experimental and DFT insights

Nitrogen-doped mesoporous graphene hydrogel (MGHG) enjoys many unique characteristics for use as an efficient energy storage electrode material. Herein, a green one-pot hydrothermal synthesis strategy was employed to synthesize highly hydrophilic nitrogen-doped mesoporous graphene hydrogel. The morphological, structural, and compositional analyses were performed using FESEM, XRD, and XPS techniques. The as-prepared MGHG exhibits high wettability (contact angle = 58.9o), high surface area (318.226 m2/g), and an unprecedented nitrogen doping content of 2.95%. The fabricated MGHG was evaluated as a supercapacitor material in 1 M aqueous K2SO4 electrolyte, revealing a maximum specific capacitance of 595.7 F.g−1 with a low equivalent series resistance (0.1664 Ω) that is ascribed to the high porosity, high surface area, and the available nitrogen redox active sites. To further elucidate the electrochemical performance of MGHG, a symmetric supercapacitor device was assembled using MGHM as negative and positive electrodes. The fabricated device shows a maximum specific energy of 30 Wh kg−1 corresponding to a specific power 1000 W kg−1. The density functional theory (DFT) computations were utilized to better understand the high performance of the assembled devices. These superior results demonstrate the excellent performance of MGHG as a potential material for highly-performing supercapacitor devices with a potential window of 2.2 V.

Boosted insights of novel accordion-like (2D/2D) hybrid photocatalyst for the removal of cationic dyes: Mechanistic and degradation pathways

In the present work, a novel (2D/2D) accordion like CS@g‒C3N4/MX hybrid composite was prepared through one-pot hydro-thermal synthesis method and utilized as a catalyst for the degradation of organic persistent dyes such as methylene blue (MB) and rhodamine B (RhB). Because the removal of such organic compounds is a major dispute in environmental aspects. In this study, the bio-assisted g‒C3N4/MX nanosheets was utilized for the removal of organic dyes from aqueous solution under visible light irradiation, respectively. The CS@g-C3N4/MX photocatalyst showed high catalytic activity based on ~99% and ~98.5% degradation of MB and RhB within 60 and 40 min using visible light irradiation. This outcome could have resulted in greater catalytic enactment towards the degradation of other persistent pollutants with enhanced light absorption property and it can efficiently suppress photo-generated charge recombination, thus improving the interfacial charge transfer rate. The OH radical was being effective oxidative species involved in the CS@g-C3N4/MX system for the degradation of organic contaminants. Furthermore, CS@g-C3N4/MX showed excellent photo-stability over five consecutive cycles for the degradation of organic dyes with negligible loss of photocatalytic activity. Finally, the purposed catalytic mechanisms and degradation pathways of MB and RhB were systematically discussed in detail based on experimental results. Thus, the organics which oxidized into ring-opened compounds such as ethoxyethane, butadiene etc., to non-toxic products like H2O, CO2 and some mineral salts.

Enhanced Friedel-Crafts benzylation activity of bimetallic WSn-KIT-6 catalysts

A series of W and Sn-containing KIT-6 mesoporous silicates (designated as WxSn5) with similar Sn (~5 wt%) and varying W (x = 3–23 wt%) loadings were prepared by a one-pot hydrothermal synthesis method. No detectable bulk WO3 species were observed for W loading up to 14 wt% with preferential dispersion of WOx species near SnO2 sites. The WxSn5 materials exhibited superior performance for Friedel-Crafts anisole benzylation with intrinsic rate constants for all WxSn5 catalysts being greater than those without Sn. Based on results from DR-UV–Vis, XRD, XPS, EXAFS techniques, we postulate that the WxSn5 materials contain both isolated [WO4]2-/SnO2 and isolated [WO4]2-/SiO2 as active species, with the former being more active. The relative populations of these two highly dispersed species dictate the overall catalyst activity. The intrinsic activities of the WxSn5 catalysts are found to scale linearly with total acidity but are mainly dictated by the Lewis acid sites.

Graphene oxide-manganese ferrite (GO-MnFe2O4) nanocomposite: One-pot hydrothermal synthesis and its use for adsorptive removal of Pb2+ ions from aqueous medium

Herein, we showed that the graphene oxide with manganese ferrite (GO-MnFe2O4) possess great adsorption properties for the selective Pb2+ ions removal from the aqueous medium. Nanocomposite adsorbent was developed by one-pot hydrothermal method, using graphene oxide as a supporting material to minimize the aggregation of MnFe2O4. Also, GO possesses important role in the adsorption mechanism of Pb2+ through electrostatic/ionic interactions. The characterizations such as FT-IR, XPS, P-XRD, FE-SEM, and BET of the synthesized nanocomposite were carried out to assess the different properties such as functionalities, crystallinity, morphology, and surface area value, respectively. Thereafter, the adsorption performance of GO-MnFe2O4 nanocomposite was tested for the Pb2+ at various adsorption parameters including to contact time, solution pH, adsorbent dose, and concentration of initial Pb2+ in order to measure the optimum adsorption condition. Kinetic experiments suggest that the equilibrium attained in 30 min and followed a pseudo-second-order kinetic model. Adsorption isotherm model followed to Langmuir isotherms and gives a maximum adsorption capacity of 621.11 mg/g. The reusability tests exhibited good durability and good efficiency for repeated Pb2+ adsorptions with GO-MnFe2O4 nanocomposite. These results demonstrated that the GO-MnFe2O4 nanocomposite may be an attractive adsorbent having low-cost for the effectively Pb+2 removal of from the polluted water.

One-pot hydrothermal synthesis of MXene Ti3C2/TiO2/BiOCl ternary heterojunctions with improved separation of photoactivated carries and photocatalytic behavior toward elimination of contaminants

Facilitating the separation rate of photoactivated carries by building of heterojunctions is a valid way to tune the photocatalytic performance. In this contribution, Ti3C2/TiO2/BiOCl ternary heterojunction photocatalysts were prepared by a hydrothermal strategy. The fabricated heterostructures were examined using diverse analysis techniques. Surface photovoltage spectrum (SPS), photocurrent response (PR) and impedance spectroscopy (IS) results reveal that the separation behavior of photoactivated carries of Ti3C2/TiO2/BiOCl ternary heterojunctions was significantly improved in contrast with the reference BiOCl. Trapping and electron spin resonance (ESR) experiments indicate that construction of heterostructures among Ti3C2, TiO2 and BiOCl is propitious to the production of O2− and OH radicals. The photocatalytic activity can be profited from the improved separation efficiency of photoinduced carries and the elevated level of active species. The photocatalytic performance of the fabricated heterostructures was assessed by disinfection of rhodamine B (RhB) and tetracycline under simulated solar illumination. The investigation illustrate that the Ti3C2/TiO2/BiOCl ternary heterojunctions display boosted photocatalytic activities than the pristine BiOCl, the 4%Ti3C2/TiO2/BiOCl holds the best decontamination ability toward RhB. Moreover, the as-prepared Ti3C2/TiO2/BiOCl ternary heterojunctions possess excellent stability even after four cycles. In view of all the observations, separation and migration mechanism of the photoinduced carriers were proposed.

TiO2 coupled to predominantly metallic MoS2 for photocatalytic degradation of rhodamine B

TiO2–MoS2 composites composed of predominantly metallic MoS2 (MoS2 (1 T)) sheets and uniform dispersed P25 nanoparticles were prepared by one-pot hydrothermal synthesis assisted with cetyltrimethyl ammonium bromide (CTAB). It was proved that the incorporation of CTAB played an important role through endowing the as-prepared composites with a high MoS2 (1 T) purity of 69% and supporting a good interfacial contact between TiO2 and MoS2. Benefiting from the advanced structure, not only light harvesting but also electron transfer of the composites for photocatalytic reaction was improved, resulting in outstanding catalytic performance and long durability for the photodegradation of dye rhodamine B. The possible growth and photocatalytic mechanism are discussed in detail. This work provides a highly efficient photocatalyst with multiple merits, such as light harvesting with broadened window, electron delivery channels with high mobility, active sites with a massive number, effective migration of photoelectron and so on. Simultaneously, it promises a potential bottom-up synthesis strategy assisted with surfactant on fabrication of MoS2 (1 T)-based composites, which will contribute to the improvement in energy and environment fields.

Simultaneous formation of Bi2O2(OH)(NO3)/BiOBr ultrathin hierarchical microspheres for effectively promoting visible-light-driven photocatalytic activity in environmental remediation

As a two-dimensional nanomaterial, bismuth oxybromide (BiOBr) have attracted tremendous interest in the area of visible-light photocatalysis since it can provide the internal electric field (IEF) through z-axis through its unique electronic band structure. However, the insufficient active sites and rapid recombination rate of charged carriers hamper the efficiency of the photocatalysis. To address these two major obstacles, an enticing strategy of constructing heterojunction was established by introducing Bi2O2(OH)(NO3) (BiON) in BiOBr with the same precursor. Through a facile one-pot hydrothermal synthesis, two Sillén-type layered photocatalysts, with intimately constructed ultrathin heterostructure, was synthesized by the co-precipitation method. In this work, the formation of Bismuth-based heterojunction for charge separation is established by the excessive bismuth nitrate, which subsequently participates with the in situ growth of ultrathin hierarchical microspheres. By attenuating the thickness of BiOBr from 20 nm to 8 nm with the aid of BiON, the photogenerated charges could migrate to the active sites through shorter charge diffusion pathway. Also, the BiOBr and BiON act as an active bridge to promote the separation of electron-hole pairs, which also brings out more active sites due to its increased specific surface area. BiON/BiOBr ultrathin hierarchical microspheres exhibited enhanced visible-light photocatalytic activity for decontaminating several types of pollutants. Besides, the activity of as-prepared BiON/BiOBr was further evaluated by inhibiting the growth of kanamycin-resistant bacteria strains. This study presents a novel strategy to incorporate the crystalline bismuth hydrate nitrate into BiOBr to form ultrathin hierarchical microspheres with high surface area for environmental remediation.

One-pot in-situ hydrothermal synthesis of CdS/Nb2O5/Nb2C heterojunction for enhanced visible-light-driven photodegradation

In-situ construction of heterojunction structure on substrate material is a feasible way to improve photocatalyst performance. Herein, we employed two-dimensional (2D) Nb2C MXene as the substrate material to construct CdS/Nb2O5/Nb2C ternary heterojunction structure by the one-pot hydrothermal synthesis method. The as-prepared photocatalyst achieved 92% removal efficiency towards carbamazepine (CBZ, model pollutant) under visible light radiation for 4 h, remarkably higher than that of pure CdS (75%), because the CdS/Nb2O5/Nb2C heterojunction structure significantly promoted electron-hole pair generation, separation and transfer. The 2D accordion-like Nb2C substrate prevented the agglomeration of photocatalysts. CdS nanoparticles and Nb2O5 nanorods grew insert Nb2C substrate, thus to strengthen the binding force between catalyst components and ensure that the Cd2+ leakage was obviously lower than the national standard of China. This work provides a feasible strategy of in-situ construction of visible-light-driven heterojunction photocatalysts on 2D MXene substrate for enhanced photocatalytic degradation of refractory organic pollutants in water.

One-pot hydrothermal synthesis of dual-emission fluorescent carbon dots for hypochlorous acid detection

In this work, we developed a dual-emission fluorescent carbon dots (CDs) using sodium citrate (SC), triethylenetetramine (TETA) and rose bengal (RB) as raw materials. Under the hydrothermal treatment, the carboxyl group in SC can crosslink with the amino group in TETA to form polymer-like intermediate by amide bond network. The RB molecule, a fluorescein derivative, lost halogen atoms under hydrothermal conditions and integrated with the skeleton structure of the network intermediate. Further dehydration and carbonization resulted in the dual-emission fluorescent CDs. Excited by ultraviolet (UV) light, the CDs exhibited blue and green luminescence centered at 440 nm and 525 nm, respectively. Due to the emission centers of these two colors showed different sensitivity to hypochlorous acid (HClO), we have designed a fluorescence assay to achieve quantitative detection of HClO. Upon addition of different concentrations of HClO to CDs solution in phosphate buffer (pH = 6), the blue emission decreased gradually while the green emission showed only a minimal decrease. By calculating the emission intensity ratio, a good linear relationship was achieved in the range of 0–17 μM, and the limit of detection was as low as 0.75 μM. The results reported here demonstrated a promising way to design organic dye modified CDs for sensing applications.

One-pot green hydrothermal synthesis of bio-derived nitrogen-doped carbon sheets embedded with zirconia nanoparticles for electrochemical sensing of methyl parathion

We report a simple, economical and green one-pot hydrothermal strategy to synthesize the bio-derived nitrogen-doped carbon sheets (ONCSs) embedded with zirconia nanoparticles (ZrO2NPs) with orange juice as carbon source and solvent. The ONCSs-ZrO2NPs composite was further applied in the decoration of glassy carbon electrode (GCE) for electrochemical sensing of methyl parathion. The orange juice-derived ONCSs with graphene-like micromorphology showed good electrical conductivity, large specific surface area, and nitrogen functional groups. They could accelerate the electron transport, provide sufficient electrolyte-electrode interface, and improve the surface wettability, thus forming a suitable microenvironment for the redox reaction of MP. The embedded ZrO2NPs in graphene-like ONCSs possessed a strong affinity toward the phosphorus groups on MP molecules, which could promote the preconcentration of MP in the interface of the fabricated sensor and electrolyte. Benefitting from the synergistic effect of ONCSs and ZrO2NPs/GCE, the ONCSs-ZrO2NPs/GCE sensor exhibited excellent peak current response towards MP with a linear detection range of 0.01–15 μg mL−1 and a low detection limit of 0.115 ng mL−1. Furthermore, the ONCSs-ZrO2NPs/GCE sensor presented good capability to investigate the MP levels in romaine and kiwifruit juices with satisfactory recoveries. This work provides a novel and green one-step approach in the development of carbon-based composite materials for high-performance MP electrochemical sensors.