H2O2 Generation Research Articles

Engineered Biomimetic Cancer Cell Membrane Nanosystems Trigger Gas-Immunometabolic Therapy for Spinal-Metastasized Tumors.

Despite great progress in enhancing tumor immunogenicity, conventional gas therapy cannot effectively reverse the tumor immunosuppressive microenvironment (TIME), limiting immunotherapy. The development of therapeutic gases that are tumor microenvironment responsive and efficiently reverse the TIME for precisely targeted tumor gas-immunometabolic therapy remains a great challenge. In this study, a novel cancer cell membrane-encapsulated pH-responsive nitric oxide (NO)-releasing biomimetic nanosystem (MP@AL) is prepared. Lactate oxidase (Lox) in MP@AL consumed oxygen to promote the decomposition of lactate, a metabolic by-product of tumor glycolysis, and the generation of H2O2, while L-arginine (L-Arg) in MP@AL is oxidized by H2O2 to generate nitric oxide (NO). For one thing, NO led to mitochondrial dysfunction in tumor cells to reduce oxygen consumption and promote the efficiency of Lox in lactate decomposition, thus reversing lactate-induced TIME; for another, NO effectively triggered immunogenic cell death, activated anti-tumor immune response and long-term immune memory, and ensured a favorable effect in the synergistic interaction with PD-L1 antibody for inhibiting tumor growth and recurrence. Therefore, a novel gas-immunometabolic therapy dual closed-loop nanosystem for enhancing tumor immunogenicity and remodeling lactate-induced TIME is established. Overall, this work will provide new ideas for gas therapy to effectively remodel the TIME to enhance cancer immunotherapy.

Indium Oxide Layer Dual Functional Modified Bismuth Vanadate Photoanode Promotes Photoelectrochemical Oxidation of Water to Hydrogen Peroxide.

The photoelectrochemical (PEC) dual-electron pathway for water oxidation to produce hydrogen peroxide (H2O2) shows promising prospects. However, the dominance of the four-electron pathway leading to O2 evolution competes with this reaction, severely limiting the efficiency of H2O2 production. Here, we report a In2O3 passivator-coated BiVO4 (BVO) photoanode, which effectively enhances the selectivity and yield of H2O2 production via PEC water oxidation. Based on XPS spectra and DFT calculations, a heterojunction is formed between In2O3 and BVO, promoting the effective separation of interface and surface charges. More importantly, Mott-Schottky analysis and open-circuit potential measurements demonstrate that the In2O3 passivation layer on the BVO photoanode shifts the hole quasi-Fermi level towards the anodic direction, enhancing the oxidation level of holes. Additionally, the widening of the depletion layer and the flattening of the band bending on the In2O3-coated BVO photoanode favor the generation of H2O2 while suppressing the competitive O2 evolution reaction. In addition, the coating of In2O3 can also inhibit the decomposition of H2O2 and improve the stability of the photoanode. This work provides new perspectives on regulating PEC two/four-electron transfer for selective H2O2 production via water oxidation.

Unveiling tomorrow: Carbonic anhydrase activators and inhibitors pioneering new frontiers in Alzheimer's disease.

Alzheimer's disease (AD) is a neurodegenerative disorder and a principal basis of dementia in the elderly population globally. Recently, human carbonic anhydrases (hCAs, EC 4.2.1.1) were demonstrated as possible new targets for treating AD. hCAs are vital for maintaining pH balance and performing other physiological processes as they catalyze the reversible hydration of carbon dioxide to bicarbonate and a proton. Current research indicates that hCA plays a role in brain functions critical for transmitting neural signals. Activation of carbonic anhydrase (CA) has emerged as a promising avenue in addressing memory loss and cognitive issues. Conversely, the exploration of CA inhibition represents a novel frontier in this field. By enhancing glial fitness and cerebrovascular health and blocking amyloid-β (Aβ)-induced mitochondrial dysfunction pathways, cytochrome C (CytC) release, caspase 9 activation, and H2O2 generation in neurons, CA inhibitors improve cognition and lessen the pathology caused by Aβ. Recent research has pushed hCAs into the spotlight as critical players in AD pathogenesis and precise therapeutic targets. The captivating dilemma of choosing between hCA inhibitors and activators looms large, as inhibitors reduce Aβ aggregation and improve cerebral blood flow, while activators enhance cerebrovascular functions and restore pH balance. The current review sheds light on the clinical evidence for hCAs and the roles of inhibitors and activators in AD. Additionally, this review offers a fascinating outlook on the data that may aid medicinal chemists in designing and developing new leads that are more effective and selective for upcoming in vitro and in vivo studies, allowing for the discovery and introduction of novel drug candidates for the treatment of AD to the market and into the clinical pipeline.

Fluorine-Doped Graphene Oxide-Modified Graphite Felt Cathode for Hydrogen Peroxide Generation

Electrochemical oxygen reduction via the two-electron pathway (2e-ORR) is an emerging method for producing H2O2. It is cleaner, safer, and more convenient compared to the anthraquinone process. Graphite felt is one of the cathode candidates for large-scale cells due to its excellent mechanical properties. However, commercial graphite felt often fails to achieve the desired hydrogen-peroxide yield because of its low catalytic selectivity for the 2e-ORR pathway. Fluorine-doped carbon materials are expected to enhance 2e-ORR selectivity. This is because the electronic structure of carbon atoms adjacent to fluorine atoms may facilitate the production of hydrogen peroxide while hindering its further reduction. In this study, fluorine-doped graphene oxide (FGO) was prepared by the hydrothermal method. Subsequently, graphite felt modified with FGO was fabricated and used as the cathode for H2O2 production. The results indicated that in alkaline media, the graphite felt modified with FGO achieved a catalytic selectivity of 93% and a generation rate of 8.91 mg cm⁻2 h⁻¹. In comparison, commercial graphite felt had a catalytic selectivity of 75% and a generation rate of 2.10 mg cm⁻2 h⁻¹. Moreover, graphite felt modified by FGO also exhibited excellent electrocatalytic performance for H2O2 generation in neutral media. This research provides a fundamental study to promote the application of graphite felt in the environmentally friendly electrocatalytic production of hydrogen peroxide in industries.

Al-N3 Bridge Site Enabling Interlayer Charge Transfer Boosts the Direct Photosynthesis of Hydrogen Peroxide from Water and Air.

Manipulating the electronic environment of the reactive center to lower the energy barrier of the rate-determining water oxidation step for boosting the direct generation of H2O2 from water, air, and sunlight is fascinating yet remains a grand challenge. Driven by a first-principles screening across a series of metal single atoms in carbon nitride, we report a class of an Al-N3 bridge site enabling interlayer charge transfer in carbon nitride nanotubes (CNNT-Al) for the highly efficient photosynthesis of H2O2 directly from water, oxygen, and sunlight. We demonstrate that the interlayered Al-N3 bridge site in CNNT-Al is able to activate the neighboring surface N atom for promoting the rate-determining step of the two-electron water oxidation to H2O2. It is also able to act as a bridge for enhancing the vertical interlaminar charge transfer due to the hybridization between the 3s and 3p states of the interstitial Al atom and the conduction band of two adjacent carbon nitride layers. Collectively, these factors lead to a highest photocatalytic mass activity of 1410.2 μmol g-1 h-1 (with a photocatalyst concentration of 1 g L-1) for direct photosynthesis of H2O2 out of all CN-based photocatalysts and a 7-fold higher solar-to-chemical conversion efficiency (0.73%) compared to that of the natural photosynthesis of typical plants (∼0.1%). Most importantly, the CNNT-Al-based flow reactor can steadily produce H2O2 for 200 h and be directly used for the on-site degradation of organic dye in water. The CNNT-Al-based flow reactor can also kill a 10 times higher concentration of bacteria in deionized water than that in natural water with 100% efficiency, which makes our design economically appealing for practical water treatment.

Additive Effects of Cu-ATSM and Radiation on Survival of Diffuse Intrinsic Pontine Glioma Cells.

Diffuse intrinsic pontine gliomas (DIPG) are highly aggressive and treatment-resistant childhood primary brainstem tumors with a median survival of less than one year after diagnosis. The prevailing standard of care for DIPG, radiation therapy, does not prevent fatal disease progression, with most patients succumbing to this disease 3-8 months after completion of radiation therapy. This underscores the urgent need for novel combined-modality approaches for enhancing therapy responses. This study demonstrates that the cellular redox modulating drug, copper (II)-diacetyl-bis(N4-methylthiosemicarbazone) (Cu-ATSM) dose-dependently (1-3 μM) decreased clonogenic cell survival in SU-DIPG50 and SU-DIPG36 cell lines during 6 h of exposure but had no significant effect on survival in normal human astrocytes (NHA). Additional significant (>90%) decreases in DIPG clonogenic survival were observed at 24 h of Cu-ATSM exposure. However, NHAs also began to show dose-dependent 10-70% survival decreases at this point. Notably, 3 μM Cu-ATSM for 6 h resulted in additive clonogenic cell killing of DIPG lines when combined with radiation, which was not seen in NHAs and was partially inhibited by the copper chelator, bathocuproinedisulfonic acid. Cu-ATSM toxicity in DIPG cells was also inhibited by overexpression of mitochondrial-targeted catalase. These results support the hypothesis that Cu-ATSM is selectively cytotoxic to DIPGs by a mechanism involving H2O2 generation and copper and being additively cytotoxic with ionizing radiation.

Continuous Electrosynthesis of Pure H2O2 Solution with Medical-Grade Concentration by a Conductive Ni-Phthalocyanine-Based Covalent Organic Framework.

Electrosynthesis of H2O2 provides an environmentally friendly alternative to the traditional anthraquinone method employed in industry, but suffers from impurities and restricted yield rate and concentration of H2O2. Herein, we demonstrated a Ni-phthalocyanine-based covalent-organic framework (COF, denoted as BBL-PcNi) with a higher inherent conductivity of 1.14 × 10-5 S m-1, which exhibited an ultrahigh current density of 530 mA cm-2 with a Faradaic efficiency (H2O2) of ∼100% at a low cell voltage of 3.5 V. Notably, this high level of performance is maintained over a continuous operation of 200 h without noticeable degradation. When integrated into a scale-up membrane electrode assembly electrolyzer and operated at ∼3300 mA at a very low cell voltage of 2 V, BBL-PcNi continuously yielded a pure H2O2 solution with medical-grade concentration (3.5 wt %), which is at least 3.5 times higher than previously reported catalysts and 1.5 times the output of the traditional anthraquinone process. A mechanistic study revealed that enhancing the π-conjugation to reduce the band gap of the molecular catalytic sites integrated into a COF is more effective to enhance its inherent electron transport ability, thereby significantly improving the electrocatalytic performance for H2O2 generation.

Visible light-driven aerobic oxidation of amines coupling with H2O2 production catalyzed by CoPc/alkali metal-doped g-C3N4 Z-scheme heterojunction

Three environmentally friendly Z-scheme CoPc/alkali metal-doped g-C3N4 heterojunction composites were fabricated via in-situ immobilizing cobalt phthalocyanine (CoPc) on the surface of alkali metal-doped g-C3N4 nanosheet by simple hydrothermal method. These composites acted as efficient and recyclable heterogeneous photocatalysts realized that the highly selective aerobic oxidation of amines to the corresponding imines coupling of hydrogen peroxide generation at room temperature. Under irradiation by LED lamp, the imines and H2O2 were obtained with conversion ranges from 87.9 % to 92.0 %, selectivity more than 99 %, and production rate ranges from 3.27 to 3.40 mmol g−1 h−1, respectively. Based on the mechanistic analysis and characterization, the excellent catalytic activity derived from the Z-scheme mechanic and synergistic effect originated from O2 reduction and amine oxidation. On completion, after centrifugation, washing with solvent and drying under vacuum, the catalysts can be recovered and reused for five successive cycles of testing with a slight decrease in reactivity. For this work, a promising photo synthesis pathway with merits of mild, low-cost, pollution-free, and energy-saving was developed to produce imines coupling with H2O2 generation.

CuO/Cu(OH)2@g-C3N4 derived from CuBTC/g-C3N4 for two channel photocatalytic hydrogen peroxide production

Photocatalytic production of H2O2 is indeed a safe, sustainable and cost-effective technology, offering an environmentally friendly solution to the energy crisis through solar photocatalysis. However, it still faces challenges such as reliance on organic electron donors and pure O2, as well as inefficiencies in hole utilization. To overcome these limitations, a dual-channel photocatalytic system has been developed. In this study, we showcase the efficiency of the CuO/Cu(OH)2@g-C3N4 composite, derived from CuBTC/g-C3N4 via NaOH treatment, as a high-performance dual-channel photocatalyst for H2O2 production. Under visible light (λ ≥ 420 nm), this composite achieves a H2O2 yield of 1354 μmol/L in 120 min without any sacrificial agent, outperforming g-C3N4 by 8.4 times, CuO by 13.6 times and CuO@g-C3N4 by 1.9 times. Quenching experiments and electron paramagnetic resonance spectra confirmed that HO• and O2•− are intermediate products in the photocatalytic process, following a two-step single-electron reaction pathway. The superior activity of CuO/Cu(OH)2@g-C3N4 in H2O2 generation can be attributed to the synergistic effects of OH bonds on the CuO@g-C3N4 Z-type heterojunction and Cu(OH)2. This research presents a straightforward and promising approach for developing highly efficient photocatalysts for energy conversion.

Electrochemical removal of imidacloprid on different anodes with in-situ H2O2 generation: Optimizing conditions for rapid degradation and safe byproducts

Electrochemical removal of imidacloprid on different anodes with in-situ H2O2 generation: Optimizing conditions for rapid degradation and safe byproducts

Electrocatalytic degradation of naphthenic acids using reduced graphene oxide modified nickel foam cathode: Role of surface structure and superoxide radical

In this work, the reduced graphene oxide (RGO) modified nickel foam (Ni-foam) was prepared via the hydrothermal reduction self-assembly method and was applied as the cathode for the effective electrocatalytic (EC) degradation of recalcitrant naphthenic acids (NAs) that are abundantly present in the petroleum industrial wastewater. The Ni@RGO cathode has greatly enhanced the production of H2O2 in the system to boost the degradation of 1-adamantanecarboxylic acid (ACA) that was a model NA compound. Results showed that the EC/Fe(III)/Ni@RGO system achieved complete ACA degradation within 15 min due to its elevated H2O2 generation and Fe(III)/Fe(II) circulation, compared to EC/Fe(III)/Ni-foam and EC/Fe(III)/Graphite systems. Interestingly, abundant ·O2– radicals, which were produced in EC/Fe(III)/Ni@RGO system as a key intermediate for 2e- oxygen reduction reaction (ORR), could effectively accelerate the circulation of Fe(III)/Fe(II) to activate H2O2 to generate ·OH for ACA degradation. Results of material characterization, electrochemical analysis and density functional theory (DFT) calculations showed that Ni@RGO cathode has obtained elevated electron transfer efficiency compared to that of Ni-foam cathode. Surface structure of RGO, such as carbon edge and vacancy with specific configuration, residual –COOH oxygenation groups on RGO surface are main catalytic sites to enhance the capacity of 2e- ORR and electron capture processes in the system. This study provides new insights regarding the synthesis process of catalytic electrodes, the influence of carbon-based material structure on catalytic activity, and the critical role of free radicals in the electro-Fenton system with Ni@RGO cathode

CaviPlasma: parametric study of discharge parameters of high-throughput water plasma treatment technology in glow-like discharge regime

Abstract AC discharge in a dense hydrodynamic cavitation cloud in water, called CaviPlasma, has been studied at different discharge parameters. CaviPlasma stands for cavitation and plasma, which are two coupled basic phenomena of the novel technology enabling very high throughput of plasma water processing compared to other current technologies. In this article, the diagnostics and the properties of CaviPlasma discharge are discussed based on optical and electric characterization of the discharge phenomena together with the physico-chemical characterization of the plasma-treated water. The so-called unbridged mode of CaviPlasma operation is described, where the discharge propagates from a metal electrode towards a liquid electrode at the collapsing end of the cavitation cloud. The production of H, O and OH species in the discharge was proven by optical emission spectroscopy. The formation of hydrogen peroxide (H2O2) in water was determined by chemical methods. The energy yield for H2O2 generation is as high as 9.6 g kWh−1 and the generation rate is up to 2.4 g h−1. The degradation of phenol admixture in water was also studied. The article covers a parametric study enabling the development of tailored applications.

Modulating Core Polarity in Metal-free Covalent Organic Frameworks for Selective Electrocatalytic Hydrogen Peroxide Production.

Tuning the charge density at the active site to balance the adsorption ability and reactivity of oxygen is extremely significant for driving a two-electron oxygen reduction reaction (ORR) to produce hydrogen peroxide (H2O2). Herein, we have highlighted the influence of intermolecular polarity in covalent organic frameworks (COFs) on the efficiency and selectivity of electrochemical H2O2 production. Different C3 symmetric building blocks have been utilized to regulate the charge density at the active sites. The benzene-cored COF, which exhibits reduced polarity than the triazine-cored COF, displayed enhanced performance in H2O2 production, achieving 93.1% selectivity for H₂O₂ at 0.4 V with almost two-electron transfer and a faradaic efficiency of 90.5%. In-situ electrochemical Raman spectroscopy and scanning electrochemical microscopy (SECM) were employed to confirm H₂O₂ generation and analyze spatial reactivity patterns. These techniques provided detailed insights into localized catalytic behavior, emphasizing the influence of core polarity.

Isolated Ni Atoms for Enhanced Photocatalytic H2O2 Performance with 1.05% Solar-to-Chemical Conversion Efficiency in Pure Water.

Photocatalytic hydrogen peroxide (H2O2) production encounters a major impediment in its low solar-to-chemical conversion (SCC) efficiency due to undesired H2O2 product decomposition. Herein, an isolated nickel (Ni) atom modification strategy is developed to adjust the thermodynamic process of H2O2 production to address the challenge. Sacrificial experiments and in situ characterization reveal that H2O2 generation occurs via a highly selective indirect two-electron oxygen reduction reaction. The optimized photocatalyst exhibits a remarkable H2O2 production rate of 338.9 μmol gcat-1 h-1 in pure water, representing a 48-fold enhancement. Notably, it attains an impressive SCC efficiency of 1.05%, surpassing that of current state-of-the-art catalysts. Theoretical insights reveal the downshifted d-band center facilitates moderate O2 adsorption and barrier-free *OOH conversion, favoring H2O2 release and preventing *H2O2 decomposition. This work showcases efficient H2O2 photosynthesis via d-band manipulation, presenting a fresh perspective for advancing high-efficiency SCC systems.

Modulating Core Polarity in Metal‐free Covalent Organic Frameworks for Selective Electrocatalytic Hydrogen Peroxide Production

Tuning the charge density at the active site to balance the adsorption ability and reactivity of oxygen is extremely significant for driving a two‐electron oxygen reduction reaction (ORR) to produce hydrogen peroxide (H2O2). Herein, we have highlighted the influence of intermolecular polarity in covalent organic frameworks (COFs) on the efficiency and selectivity of electrochemical H2O2 production. Different C3 symmetric building blocks have been utilized to regulate the charge density at the active sites. The benzene‐cored COF, which exhibits reduced polarity than the triazine‐cored COF, displayed enhanced performance in H2O2 production, achieving 93.1% selectivity for H₂O₂ at 0.4 V with almost two‐electron transfer and a faradaic efficiency of 90.5%. In‐situ electrochemical Raman spectroscopy and scanning electrochemical microscopy (SECM) were employed to confirm H₂O₂ generation and analyze spatial reactivity patterns. These techniques provided detailed insights into localized catalytic behavior, emphasizing the influence of core polarity.

Perfect Is Perfect: Nickel Prussian Blue Analogue as A High‐Efficiency Electrocatalyst for Hydrogen Peroxide Production

AbstractPrussian blue analogues (PBA) are a large family of functional materials with diverse applications such as in electrochemical fields. However, their use in the emerging two‐electron oxygen reduction reaction for clean production of hydrogen peroxide (H2O2) is lagging. Herein, a general solvent exchange induced reconstruction strategy is demonstrated, through which an abnormal NiNi‐PBA superstructure is synthesized as a high‐performance electrocatalyst for H2O2 generation. The resultant NiNi‐PBA superstructure has a stoichiometric composition with saturated lattice water, and a leaf‐like morphology composed of interconnected small‐size nanosheets with identical orientation and predominate {210} side surface exposure. Our studies show that the Ni−N centers on {210} facets are the active sites, and the saturated lattice H2O favors a six‐coordinated environment that results in high selectivity. The “perfect” structure including stoichiometric composition and ideal facet exposure leads to a high selectivity of ~100 % and H2O2 yield of 5.7 mol g−1 h−1, superior to the reported MOF‐based electrocatalysts and most other electrocatalysts.

Phosphate-Induced Acidic Microenvironment for Improved Contaminant Removal during FeS Oxygenation.

The coexistence of mackinawite (FeS) and phosphate is widely observed in natural systems. However, the underlying mechanism regarding how phosphate influences the environmental behavior of FeS, especially during the FeS oxygenation in aquatic systems, remains in its fancy. This study for the first time reported that the presence of phosphate, even at a low concentration of 0.3 mM, significantly promoted the FeS-mediated O2 activation and thus the pollutant degradation. The enhancement was attributed to a substantial increase in the generation of •OH, as evidenced by the electron paramagnetic resonance tests and the identification of the probing products. A combination of experiments and theoretical calculations revealed that phosphate adsorbed onto the FeS surface via a monodentate mononuclear configuration, establishing an acidic microenvironment on the FeS surface. Such acidic microenvironment not only increased the utilization efficiency of Fe(II) toward H2O2 generation (i.e., ), but also prevented the subsequent side reaction of H2O2 self-decomposition (i.e., ). The results highlight the beneficial role of commonly encountered phosphate in FeS-based systems, which has profound implications for the degradation of waterborne contaminants.

Undervalued role of metal-carbon junction in selective generation of H2O2: An example of the zinc-carbon junction edge providing asymmetric active sites for efficient oxygen reduction

The spontaneous oxygen reduction is a potential technology for in-situ H2O2 production, which gets rid of the dependence on electricity and solar energy. Previous some metal–carbon compounds reported are feasible to trigger oxygen reduction. These reports always claim the high H2O2 generation ability of metal–carbon composites, while rarely discuss the contribution of carbon and the carbon–metal junction to the oxygen reduction process. Inspired by the dual active sites, we infer that the role of interfacial carbon in metal–carbon composites is underestimated. By a heat treatment of the co-precipitate of zinc and glucose, the Zn-C junction is constructed in Zn-gc to achieve a spontaneous selective reduction of O2 to H2O2. The Zn-C interface edge is active site, where an asymmetric activation is achieved by bonding two O atoms from O2 to C and Zn, respectively. The Zn traction to one of the O atoms is mainly in xy plane, while the C traction to the other O atom is parallel to z-axis. The yield of H2O2 produced per gram of Zn increases from 27.89 mg to 122.21 mg, an improvement of 4.38 times. And the inertness of Zn and its oxygen-containing compounds towards H2O2 enables Zn-gc/O2 system to stabilize H2O2 over a long period of time. This work reveals the crucial role of neglected junction interfaces in oxygen reduction reactions in metal–carbon composites.

Modelling and optimization of amoxicillin degradation over ZnO and glucose oxidase modified TiO2 nanowire

AbstractRecently, antibiotics posing threats to health and the environment have been highlighted. According to previous reports, amoxicillin is the most hazardous antibiotic in Tehran. In order to overcome the risks associated with the storage and contamination of oxidizing agents, a Janus structure of Ti/TiO2/FA/GOx/ZnO is introduced for in situ steady generation and consumption of H2O2. The most efficient nanowire structure of TiO2 is achieved at 140°C and 4.5 h. The footprints of GOx as the bioactive site to produce H2O2 and ZnO as the photoactive site to dope TiO2 have been proved by Raman, Fourier transform infrared (FTIR), X‐ray diffraction (XRD), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) analyses. For the first time, a Minimum Run Resolution V screening has been implemented for seven factors in an amoxicillin degradation process by the so‐called bio‐photo‐catalyst. According to analysis of variance (ANOVA), the significance of the three most important variables is as follows: amoxicillin concentration (C) > the area covered by TiO2 nanowires (E) > ZnO/GOx (F) ratio. The significance of the model over the 95% confidence interval is confirmed by R2 of 0.9970, F‐value of 108.10.

Design of dual-defective polymeric carbon nitride with compact interlayer stacking for boosting photocatalytic H2O2 production: Insight of various configurations

Polymeric carbon nitride (PCN) is an environmentally friendly photocatalyst for solar-driven H2O2 production, but the activity of original PCN is still not satisfactory. The main limitation is the sluggish exciton dissociation leading to slow generation and conversion of superoxide radical (•O2−) intermediate. Herein, the PCN with dual defect sites and compact interlayer is rationally designed for H2O2 photosynthesis with an ultrahigh rate of 3930.9 μmol g−1h−1 and rapid •O2− yield rate of 1.92 min−1. The enhanced activity is attributed to effective exciton dissociation during interlayer and intralayer process. Moreover, nitrogen vacancies change the oxygen adsorption configuration (formation of C − O − O − C bridge mode), thus promoting O2 adsorption and activation. A well-matched linear relationship was established between the concentration of nitrogen vacancies and •O2−/H2O2 production. This work not only provides in-depth insights for the photocatalytic H2O2 generation mechanism, but also offers a new paradigm for designing efficient PCN-based photocatalysts for energy conversion.