Surface Oxygen-containing Groups Research Articles

Stimulus-responsive room-temperature phosphorescence with tunable color for time-resolved advanced dynamic anti-counterfeiting

Multi-stimuli responsive multicolored room-temperature phosphorescent (RTP) carbon quantum dots (CQDs) have recently attracted considerable attention, owing to their potential applications in advanced dynamic anti-counterfeiting. The design and development of carbon dots that exhibit both stimulus response characteristics and multicolor RTP emission remains a significant challenge in the field. In this work, we present a novel approach to control the dynamic phosphorescence color and stimulus response properties of CQDs coated on paper by fine-tuning the surface functional groups of the CQDs. Specifically, histidine and 2,4,6-triaminopyrimidine was separately used to prepare N, O co-doped CQDs (NOCQDs) and N-doped CQDs (NCQDs), respectively. These CQDs were further coated on filter paper substrates to achieve water and heating cascade stimulus–response RTP. These stimuli-responsive properties of NOCQDs can be modulated by deprotonating their surface oxygen-containing groups. Eventually, we achieved time-resolved multicolor dynamic anti-counterfeiting by exploiting the stimuli-response properties and lifetimes differences between NOCQDs and NCQDs, realizing the 5D information encryption in all five stimulus-, pattern-, time-, and color-dependent codes. These findings highlight the potential of NOCQDs as advanced anti-counterfeiting materials and lay a foundation for further exploration into the synthesis and properties of CQDs with tunable stimuli-response features and RTP emission.

Temporal changes in the mobility of As, Pb, Zn, and Cu due to differences in biochar stability caused by lignin content

Understanding biochar aging is a critical factor in predicting its long-term effects when added to soil. This study explores the complex links between lignin content in biochar feedstock and biochar stability during accelerated aging, including its influence on heavy metal mobility in soil. In this study, nine types of biochar based on fir (F), pine (P), and oak (O) sawdust were produced at 400 °C, and lignin was extracted from them using ammonia after 0, 3, and 7 days (named as 0FB, 3FB, 7FB, 0 PB, 3 PB, 7 PB, 0OB, 3OB, and 7OB). Subsequently, each biochar was subjected to 25 cycles of wet-dry (WD) and freeze–thaw (FT) aging. The aged low-lignin biochars (7FB, 7 PB, and 7OB) released more dissolved organic matter (DOM) and contained more oxygen-containing surface groups on their surfaces than the high-lignin biochars (0FB, 0 PB, and 0OB). The low-lignin biochars with high DOM leaching released 37–85 % more anionic arsenic (As) from biochar-amended soil after 25 cycles of aging than the high-lignin biochars. The stabilities of lead (Pb), zinc (Zn), and copper (Cu) were increased due to strong binding to surface functional groups on the low-lignin biochar. The acid-soluble fractions of Pb, Zn, and Cu were converted to organic-bound fractions as biochar aging progressed, with the degree of transformation being inversely proportional to the lignin content of biochar. This research highlights the crucial role of lignin in shaping biochar stability, and reveals how biochar stability impacts soil heavy metals speciation, opening new avenues for effective biochar-based environmental solutions and the promotion of soil health.

Electric-field enhanced three-dimensional flexible carbon felt as a host for Pt4+ ions extraction

The extraction of the precious metal Pt4+ ions from aqueous solution are of great importance for both economic development and environmental protection. In this study, an electric field assisted adsorption process with high efficiency and recyclability was explored in a self-made device using three-dimensional (3D) flexible carbon felt (FCF) as the adsorbent without using conductive adhesive. Under the aid of an electric field (0.4 V), 3D pristine FCF (p-FCF) showed a considerable adsorption capacity for Pt4+ (82 mg/g). As high as 203 mg/g was obtained when o-NFCF adsorbents modified with N doping and surface oxygen-containing groups was used. Kinetic and thermodynamic studies show that the electric field would enhance the interactions between the adsorbent and Pt4+ ions, and improve the intraparticle diffusions. Mechanism study showed that the synergistic effect between N doping and oxygen-containing groups might efficiently tune the electrochemical properties of 3D FCF materials, which significantly contributed to the enhanced adsorption of Pt4+. The electroadsorption technology developed in this study provides a simple and efficient method for industrial recovery of precious metal ions.

Effect of oxidant concentration on the microwave properties of oxidized carbon fibers

Here, we report how the oxidation of carbon fibers (CFs) with H2O2 and HNO3 affects the CFs’ microwave properties. The CFs were characterized by SEM and TEM, and oxygen-containing surface groups were quantified by thermal analysis methods. Treatment with H2O2 and HNO3 solutions increased the oxygen content to about 6 at% and up to 10 at%, respectively, which decreased the reflection loss and increased the transmission loss at 25.86–37.5 GHz. The microwave properties showed pronounced correlations with the concentration of HNO3 and not with H2O2, indicating that the HNO3 oxidant is more promising for microwave loss tuning.

0D/2D Bi2MoO6 quantum dots /rGO heterojunction boosting full solar spectrum-driven photothermal catalytic CO2 reduction to solar fuels

The photothermal-catalyzed CO2 reduction is severely limited by the low carrier transport capacity. In this paper, the in-situ construction of 0D/2D Bi2MoO6 (BMO)/reduced Graphene Oxide (rGO) heterojunction was synthesized. The excellent photothermal conversion ability of rGO promotes the high dispersion of BMO quantum dots (QDs). The size of synthesized BMO QDs is about 4.26 nm and the temperature of the catalysts can quickly rise to 68.0 °C. XPS results show that the C–O–Bi interfacial electronic bridge between surface oxygen-containing groups and BMO QDs was successfully induced by modulating the degree of GO reduction. Electrons generated by BMO QDs migrate to the rGO surface rapidly, inducing rGO as a new electron-rich surface for rapid activation of CO2. The 1:5 BMO/rGO (NaBH4) CO yield reaches 186.87 μmol/g, which is 4.64 times as much as BMO QDs.

Effect of I- ligand and surface oxygen-containing groups on catalytic activity and stability of activated carbon-supported Pd catalysts in acetylene dicarbonylation

The support and ligand play a crucial role in regulating the catalytic performance, selectivity, and stability of heterogeneous catalysis. Herein, activated carbon (AC) supported palladium (Pd) catalysts (2.0 wt%) were prepared by impregnation for acetylene dicarbonylation. The oxygen-containing groups on the surface of the AC support were modulated by nitric acid (HNO3) to investigate metal–support interactions on the catalytic performance and stability of the Pd/AC. The characterization of the chemical composition and structure of the supports and catalysts demonstrates that high concentrations of oxygen-containing groups on the surface of the carbon support lead to the fine dispersion of Pd nanoparticles. Notably, the finely dispersed Pd/AC70 catalyst exhibited good activity and stability for acetylene dicarbonylation under high-pressure CO conditions after several rounds of regeneration. Furthermore, operational parameters including the type of support, co-catalyst (KI), and reaction time and temperature were identified for their impact on the reaction. It was found that I- anions serve as a co-catalyst and can ligate with Pd species, thereby preventing the leaching of Pd and improving reaction selectivity. This study presents a straightforward and sustainable modulation strategy to improve the dispersion of active metals, as well as to prevent the leaching and sintering of these metals during high-pressure CO reactions.

Contributions of surface roughness and oxygen-containing groups to the interfacial shear strength of carbon fiber/epoxy resin composites

Contributions of surface roughness and oxygen-containing groups to the interfacial shear strength of carbon fiber/epoxy resin composites

Comparative Effects of Hydrazine and Thermal Reduction Methods on Electromagnetic Interference Shielding Characteristics in Foamed Titanium Carbonitride MXene Films.

The urgent need for the development of micro-thin shields against electromagnetic interference (EMI) has sparked interest in MXene materials owing to their metallic electrical conductivity and ease of film processing. Meanwhile, postprocessing treatments can potentially exert profound impacts on their shielding effectiveness (SE). This work comprehensively compares two reduction methods, hydrazine versus thermal, to fabricate foamed titanium carbonitride (Ti3CNTx) MXene films for efficient EMI shielding. Upon treatment of ≈ 100µm-thick MXene films, gaseous transformations of oxygen-containing surface groups induce highly porous structures (up to ≈ 74.0% porosity). The controlled application of hydrazine and heat allows precise regulation of the reduction processes, enabling tailored control over the morphology, thickness, chemistry, and electrical properties of the MXene films. Accordingly, the EMI SE values are theoretically and experimentally determined. The treated MXene films exhibit significantly enhanced SE values compared to the pristine MXene film (≈ 52.2dB), with ≈ 38% and ≈ 83% maximum improvements for the hydrazine and heat-treated samples, respectively. Particularly, heat treatment is more effective in terms of this enhancement such that an SE of 118.4dB is achieved at 14.3GHz, unprecedented for synthetic materials. Overall, the findings of this work hold significant practical implications for advancing high-performance, non-metallic EMI shielding materials.

Contribution of surface roughness and oxygen-containing groups to the interfacial shear strength of carbon fiber/epoxy resin composites

The interfacial shear strength (IFSS) between carbon fibers (CFs) and the matrix is crucial to the performance of CF-reinforced polymer composites. To evaluate the contribution of mechanical interlocking and chemical anchoring at the interfaces of a polyacrylonitrile-based CF (TORAYCA T800SC-12000-10E)-reinforced epoxy resin (EP: bisphenol A type epoxy resin and tetrafunctional epoxy resin) composites, the surface roughness and content of oxygen-containing functional groups of the CFs were respectively altered by ammonia treatment and electrochemical oxidation. The results showed that ammonia treatment increased the surface roughness without much change to the surface elemental composition, while electrochemical oxidation increased the number of surface oxygen groups without changing the surface roughness. The IFSS of CF/EP composites was tested by the micro-droplet method. The relationships between IFSS, and surface roughness and oxygen content were obtained by linear fitting. The results showed that in the interfacial bonding of CF to epoxy resin, the contribution of chemical anchoring to the IFSS is larger than that of mechanical interlocking.

Persulfate activation using leonardite char-supported nano zero-valent iron composites for styrene-contaminated soil and water remediation

Effective in-situ technology to treat carcinogenic compounds in contaminated areas poses a major challenge. Our objective was to load nano-zero-valent iron (nZVI) onto leonardite char (LNDC), an alternative carbon source from industrial waste, for use as a persulfate (PS) activator for styrene treatment in soil and water. By adding a surfactant during synthesis, cetyltrimethylammonium bromide (CTAB) promotes a flower-like morphology and the nZVI formation in smaller sizes. Results showed that nZVI plays a crucial role in PS activation in both homogeneous and heterogeneous reactions to generate reactive oxygen species (ROS), which can remove 98% of styrene within 20 min. Quenching experiments indicated that singlet oxygen (1O2), superoxide radicals (O2•–), and sulfate radicals (SO4•–) were the main species working together to degrade styrene. XPS analysis also revealed a role of surface oxygen-containing groups (i.e., CO, C–OH) in activating PS for SO4•– and 1O2 generation. The possible reaction mechanism of PS activation by LNDC-CTAB-nZVI composite and factors affecting treatment efficiency (i.e., PS concentration, catalyst dosage, pH, and humic acid) were illustrated. The molarity/molality ratio of PS to nZVI should be set greater than 1 for effective styrene removal. GC-MS analysis showed that styrene was degraded to a less toxic benzaldehyde intermediate. However, the excessive use of PS and catalysts can harm plant growth, requiring a combining approach to achieve safer use for real applications. Overall results supported the use of the LNDC-CTAB-nZVI/PS system as an efficient in-situ treatment technology for soil and water remediation.

Optimization of multiscale structure and electrochemical properties of bamboo-based porous activated biochar by coordinated regulation of activation and air oxidation

Activated biochar prepared by a single pyrolysis process often has poor pore structure and insufficient surface oxygen-containing groups, which severely inhibit its application in supercapacitors. Herein, we synthesized bamboo-based porous activated biochar (PAB) via coordinated regulation including carbonization at 450 °C, ZnCl2 activation at 400 ∼ 800 °C, and air oxidation at 200 ∼ 350 °C. The results showed that the coordinated regulation could efficiently improve the physicochemical structure and electrochemical properties of PAB. Air oxidation exhibited an obvious improving effect on the activated carbon prepared with mid-temperature activation (optimal at 600 °C), which was strengthened with increasing oxidation temperature from 200 °C to 350 °C. Air oxidation following 600 °C activation could improve the mesoporous rate by etching the pore, and simultaneously introduce more oxygen-containing groups such as carbonyl (C=O) and carboxyl (–COOH) groups, which could enhance the wettability of PAB. The optimal synergistic temperature of ZnCl2 activation and air oxidation was 600 °C and 350 °C (PAB-600-350), respectively. PAB-600-350 is a wonderful supercapacitor electrode material with a higher surface oxygen content (20.74%) and a superior mesoporous rate (35%). At 1 A/g, PAB-600-350 showed the highest capacitance of 256 F/g, which was 2-fold that of PAB-600 (128 F/g). PAB-600-350 capacitors also supplied an excellent energy density of 12.54 Wh/kg at the power density of 225 W/kg in 1 M Na2SO4 electrolyte. Furthermore, a density functional theory (DFT) analysis was performed to investigate the interaction between PAB and electrolyte ions. The results showed that oxygen-containing functional groups on the surface can increase the dipole moment of the material and enhance the adsorption of PAB for electrolyte ions (K+).

Co-doped metal–organic framework MIL-125(Ti) derivate for efficient adsorption of tetracycline hydrochloride from water

Metal-organic framework (MOF) based materials have aroused much research interest owing to their unique structural features in the field of environmental purification. Herein, a MOF derivate of Co-MIL-300 was prepared by sintering the cobalt-modified MIL-125(Ti) (Co-MIL) precursor at 300 °C in an air atmosphere and used as adsorbent to remove tetracycline hydrochloride (TCH, a typical emergent pollutant) from water. The Co-MIL-300 adsorbent possesses a large specific surface area, the rich surface oxygen-containing groups, the benzene-ring structure with rich π-electrons and surface cobalt ions benefiting for TCH adsorption. The TCH adsorption on Co-MIL-300 satisfies the pseudo-second-order kinetic model and Langmuir mode well, and is found to be a spontaneous endothermic and monolayer chemical adsorption process based on covalent bonding (such as π-π conjugation interactions, hydrogen bonding, π-cation interactions, coordination bonding) adsorption mechanism. Co-MIL-300 reveals a much higher adsorption capacity than Co-MIL (2.3 times of the latter) with qmax = 321.5 mg⋅g−1 at 30 °C, and it also keeps a high adsorption capacity in a wide pH range (pH = 2–11). The coexisting CO32–, PO43-, Al3+ and Fe3+ ions can greatly inhibit TCH adsorption. Most of its adsorption capacity can be recovered in five cycles after regeneration, showing great application potential for antibiotics removal.

Molybdenum disulfide (MoS2)/porous silica nanosheet composite barrier for polysulfide shuttling inhibition in lithium-sulfur batteries

Lithium-sulfur batteries (LSBs) is the key choice for the next generation of high energy density batteries, while the shuttle effect of polysulfides greatly limits its development. Constructing a multifunctional barrier layer has been proved to be an effective method to inhibit the shuttle of polysulfides. Herein, molybdenum disulfide (MoS2)/2D porous silica nanosheets (PSN) composite is designed as the barrier layer. The surface oxygen-containing groups on both PSN and MoS2 enhance the adsorption for LiPSs, and the MoS2 plays a role of catalyst to facilitate the rapid polysulfide transformation. Meanwhile the abundant pores of PSN guide the uniform deposition of lithium on lithium metal anode, finally realizing the efficient transformation of lithium polysulfides and inhibition of lithium dendrites. The LSBs based on the MoS2/PSN barrier deliver high initial discharge capacity of 1521 mAh g−1 at 0.1 C, low decay rate of 0.056% per cycle at 2 C over 600 cycles, and outstanding rate performance with a high discharge capacity of 649 mAh g−1 at 4 C. The corresponding pouch cells show high discharge capacity and cycling stability, further demonstrating the potential application of the composite barrier in high-energy-density LSBs.

Functional Group Modulation in Carbon Quantum Dots for Accelerating Photocatalytic CO2 Reduction.

This study investigates the mechanism behind the enhanced photocatalytic performance of carbon quantum dot (CQD)-induced photocatalysts. Red luminescent CQDs (R-CQDs) were synthesized using a microwave ultrafast synthesis strategy, exhibiting similar optical and structural properties but varying in surface functional group sites. Model photocatalysts were synthesized by combining R-CQDs with graphitic carbon nitride (CN) using a facile coupling technique, and the effects of different functionalized R-CQDs on CO2 reduction were investigated. This coupling technique narrowed the band gap of R1-CQDs/CN, made the conduction band potentials more negative, and made photogenerated electrons and holes less likely to recombine. These improvements greatly enhanced the deoxygenation ability of the photoinduced carriers, increased light absorption of solar energy, and raised the carrier concentration, resulting in excellent stability and remarkable CO production. R1-CQDs/CN demonstrated the highest photocatalytic activity, with CO production up to 77 μmol g-1 within 4 h, which is approximately 5.26 times higher than that of pure CN. Our results suggest that the superior photocatalytic performance of R1-CQDs/CN arises from its strong internal electric field and high Lewis acidity and alkalinity, attributed to the abundant pyrrolic-N and oxygen-containing surface groups, respectively. These findings offer a promising strategy for producing efficient and sustainable CQD-based photocatalysts to address global energy and environmental problems.

Constructing the quinonyl groups and structural defects in carbon for supercapacitor and capacitive deionization applications

The structural defects and oxygen-containing functional groups of carbon materials as electrode materials for supercapacitors or capacitive deionization devices are critical to their electrochemical performance. The tuning of surface oxygen-containing functional groups and carbon defects during pyrolysis is key to achieve a high performance in ion storage. Herein, quinonyl-dominant defective porous carbon is prepared by a pyrolysis and cross-linking route using lavender stem and potassium acetate as precursor. Benefiting from the presence of abundant defect and surface quinonyl groups, porous carbon shows an ultra-high specific capacitance of 401 F g−1 (1 A g−1) and a high capacitance retention of 63% at a high current density of 100 A g−1 in a KOH solution. Meanwhile, as a capacitive deionization electrode material, it also exhibited a high adsorption capacity of 25.5 mg g−1 in 500 mg L-1 NaCl solution at 1.2 V. Theoretical density functional theory (DFT) calculation demonstrates that surface quinonyl groups and carbon defects can synergistically facilitate the adsorption of K+ and Na+ during the charge/discharge process. This work provides a new perspective for understanding the role of surface oxygen-containing groups and intrinsic defects of porous carbon materials in electrochemical energy storage and desalination applications.

Sludge-based activated biochar for adsorption treatment of real oil sands process water: Selectivity of naphthenic acids, reusability of spent biochar, leaching potential, and acute toxicity removal

Large volumes of oil sands process water (OSPW) containing naphthenic acids (NAs) and other contaminants are generated by oil sands operations. For the first time, pristine and zinc chloride-activated biochars from sludge from a municipal wastewater treatment plant are studied in the adsorption of NAs in real OSPW. By using activated biochar instead of pristine biochar, the adsorption capacity (qt) for total NAs (classical and oxidized NAs) increased from 2.3 to 26.6 mg/g. The increase in qt for activated biochar was related to the improvement of surface area from 7.9 to 513 m2/g, the abundance of mesopores (89% of pore volume), and the oxygen-containing surface groups. Equilibrium was reached at 2 h of contact time. Considering the thousands of structures of NAs in the OSPW, the activated biochar presented higher affinity for NAs with higher carbon and double bond equivalency numbers, therefore, NAs with more hydrophobic and higher cyclicity characteristics. Pore-filling, hydrogen bonding, and π-π interactions are the adsorption mechanisms. Thermal regeneration of spent activated biochar was studied, and in the fifth cycle of regeneration, the regenerated biochar had qt of 7.1 mg/g, which was 5 times higher than the adsorption capacity of fresh pristine biochar. Adsorption treatment of OSPW using activated biochar decreased the following parameters: metals Mg (7%), Ca (21%), Sr (27%), and Ba (60%), organic matter by means of DOC (63%) and COD (66%), acute toxicity towards V. fischeri (66%) and bioavailability of organics (91%). These findings promote circular economy as it presents an efficient adsorbent for NAs in OSPW developed from sludge, reducing the environmental impact associated with sludge disposal and allowing the efficient reclamation and reuse of OSPW.

Boron-Doped and Ketonic Carbonyl Group-Enriched Graphdiyne as a Dual-Site Carbon Nanozyme with Enhanced Peroxidase-Like Activity.

We demonstrate the preparation of a dual-site carbon nanozyme, boron-doped and ketonic carbonyl (-C=O) group-enriched graphdiyne (B-GDY), with an enhanced peroxidase-like activity. Taking advantage of acidic oxidation treatment, GDY oxide (GDYO) with abundant surface oxygen-containing groups is obtained from pristine bulk GDY. Upon further thermal annealing of GDYO with H3BO3 under an inert atmosphere, B is introduced into GDY, while the loading of -C=O groups is increased onto B-GDY. We discover that boron-doped and ketonic carbonyl group-enriched graphdiyne as a dual-site carbon nanozyme endows it with an enhanced peroxidase-like activity, which is nearly 4.2-fold higher than that of GDY without B atoms and 6.6-fold higher than that of GDYO without B atoms and with low loading of -C=O groups. The high peroxidase-like activity of B-GDY is ascribed to the dual active sites (-C=O group and B atom) within it, which facilitates the adsorption and decomposition of H2O2 into hydroxyl radicals revealed by experimental and theoretical studies. Moreover, B-GDY is successfully employed to develop a colorimetric method for the detection of glucose with good sensitivity and selectivity. This work probes into the intrinsic peroxidase activity and structure-reactivity correlation, creating effective strategies for the preparation of GDY-based nanozymes.

Cerium-Bismuth Oxides/Oxynitrates with Low Toxicity for the Removal and Degradation of Organophosphates and Bisphenols.

Nanoscale cerium-bismuth oxides/oxynitrates were prepared by a scalable low-temperature method at ambient pressure using water as the sole solvent. Solid solutions were formed up to a 1:1 Ce/Bi molar ratio, while at higher doping levels, bismuth oxynitrate photocatalysts with a pronounced layered structure were formed. Bismuth caused significant changes in the structure and surface properties of nanoceria, such as the formation of defects, oxygen-containing surface groups, and Lewis and Brønsted acid sites. The prepared bifunctional adsorbents/photocatalysts were efficient in the removal of toxic organophosphate (methyl paraoxon) from water by reactive adsorption followed by photocatalytic decomposition of the parent compound and its degradation product (p-nitrophenol). Bi-doped ceria also effectively adsorbed and photodegraded the endocrine disruptors bisphenols A and S and outperformed pure ceria and the P25 photocatalyst in terms of efficiency, durability, and long-term stability. The very low toxicity of Bi-nanoceria to mammalian cells, aquatic organisms, and bacteria has been demonstrated by comprehensive in vivo/in vitro testing, which, in addition to its simple "green" synthesis, high activity, and durability, makes Bi-doped ceria promising for safe use in abatement of toxic chemicals.

Green synthesis of surface-group-tunable red emissive carbon dots and their applications for Fe3+ and pyrophosphate detection

Red emission carbon dots (R-CDs) have great potential applications in optical and electronic devices, but few studies have focused on synthesizing R-CDs with tunable functional groups. In this study, p-phenylenediamine and hydroquinone were selected as precursors with specific hybridized carbon structures for synthesizing R-CDs with tunable functional groups by hydrothermal method. The proportion of precursors in the reaction system were adjusted to successfully synthesize R-CDs with various contents of oxygen and amino groups. Experimental results showed that the fluorescence of the R-CDs was effectively quenched by Fe3+ through the formation of R-CDs/Fe3+ complex. The fluorescence quenching ability of Fe3+ for R-CDs with different N/O ratios were also investigated. The fluorescence quenching efficiency of Fe3+ for R-CDs increased with the oxygen content of the R-CDs. By selecting R-CDs with oxygen-containing surface groups (R-O-CDs) as nanoprobe, an “on–off-on” fluorescent sensor has been developed for dual-detection of Fe3+ and pyrophosphate (PPi). A detection limit of 0.527 μM for Fe3+ and 0.24 μM for PPi were achieved. The as-developed R-O-CDs/Fe3+ nanoprobe was also successfully used to detect Fe3+ and PPi in real samples. Furthermore, an IMPLICATION logic gate was designed.

Magnetically-separable cobalt catalyst embedded in metal nitrate-promoted hierarchically porous N-doped carbon nanospheres for hydrodeoxygenation of lignin-derived species

The creation of non-noble metal magnetically-separable heterogeneous catalysts for the hydrodeoxygenation of biomass to value-added products has received substantial attention. Herein, we report a facile synthesis of magnetically-separable cobalt catalyst embedded in hierarchically porous N-doped carbon nanospheres (Co@NC) by in situ non-noble metal nitrate-promoted pyrolysis reduction strategy using nitrogen/oxygen co-doped resin polymer spheres as precursors. The facile H2O2 post-treatment process increased surface oxygen-containing groups and improved hydrophilicity to disperse catalysts in aqueous solutions. Moreover, owing to the non-noble metal nanoparticles coated with a graphitic nitrogen-doped carbon layer, the as-prepared Co@NCH2O2 catalyst exhibits excellent catalytic activity and stability of vanillin hydrodeoxygenation in aqueous solutions. This strategy can be extended to other non-noble metal nitrates like M@NCH2O2 (M = Co, Ni) within good recyclability, magnetically-separable ability, and general applicability for a broad substrate scope, further highlighting the superiority of our active catalysts.