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Materials for Hydrogen Peroxide Production via Photocatalysis

Feng Li , Qingyun He , Fang Li , Xiaolong Tang , Changlin Yu

Progress in Chemistry ›› 2023, Vol. 35 ›› Issue (2) : 330 -349.

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Progress in Chemistry ›› 2023, Vol. 35 ›› Issue (2) : 330-349 DOI: 10.7536/PC220718
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Materials for Hydrogen Peroxide Production via Photocatalysis
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Abstract

Hydrogen peroxide (H2O2) is a promising energy carrier and an environmentally friendly oxidant which is widely used in industry and health fields including organic synthesis, drinking water treatment, wastewater treatment and medical hygiene. With the promotion of environmental protection requirements, the demand for H2O2 is expected to increase substantially. H2O2 production by the traditional anthraquinone method (AQ) has a tedious process and pollutes the environment with a large amount of organic matter. In contrast, photocatalytic H2O2 production technology is a green process which uses O2 and H2O as raw materials, solar energy as energy source, and semiconductor as photocatalyst, with some distinct advantages, e. g, mild reaction conditions, simple and controllable operation, and no secondary pollution. Nowadays, the production of H2O2 via photocatalytic route has attracted extensive attention. This review introduces the mechanism of photocatalytic H2O2 production and the reasons for its low efficiency. The typical photocatalyst systems and strategies for enhancing photocatalytic efficiency in H2O2 production are intensively summarized and discussed. Finally, the perspective for the future development of photocatalytic H2O2 production is proposed.

Contents

1 Introduction

2 The mechanism of photocatalytic H2O2production and the reason for its low selectivity

3 Photocatalytic H2O2production materials

3.1 g-C3N4

3.2 Metal oxide

3.3 Transition metal sulfide

3.4 Organic framework

4 Modification strategies for photocatalyst materials

4.1 Morphology optimization

4.2 Defective engineering

4.3 Heterojunction engineering

4.4 Metal nanoparticles loading

4.5 Element doping

4.6 Introduction of quantum dot modification

4.7 Introduction of organic molecule or group

4.8 Construction of three phase reaction system

5 Conclusion and outlook

Graphical abstract

Keywords

Photocatalytic / Hydrogen peroxide / Materials / Performance enhancements / Strategies

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Feng Li, Qingyun He, Fang Li, Xiaolong Tang, Changlin Yu. Materials for Hydrogen Peroxide Production via Photocatalysis. Progress in Chemistry, 2023, 35(2): 330-349 DOI:10.7536/PC220718

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1 Introduction

Hydrogen peroxide, commonly known as hydrogen peroxide (H2O2), is the cleanest green oxidant. It has the highest content of active oxygen (47.1% w/w), and does not produce toxic by-products during the reaction, only H2O and O2[1,2]. In addition, the energy density of H2O2 is 3.0 MJ·L-1(60 wt%H2O2) higher than that of compressed hydrogen (35 MPa,2.8 MJ·L-1), which is a green storable and transportable fuel and can be directly used to generate electricity[3]. Therefore, H2O2 is widely used in the fields of organic synthesis, drinking water treatment, wastewater treatment and health care[4][5][6][7]. In recent years, the market demand for H2O2 has been rising, and it is estimated that China's demand will reach 23.79 million tons by 2025[8]. On the other hand, with the rapid consumption of fossil fuels, the conversion of solar energy into chemical energy, which is easy to store, has attracted much attention[2].
At present, H2O2 is mainly produced by anthraquinone process (AQ), which includes hydrogenation, oxidation, extraction and recycle[9]. Although it is easy to produce in batches, it consumes a lot of energy, needs to use toxic organic raw materials and solvents, and pollutes the environment seriously, so it does not meet the development requirements of green chemical production. The common alternative method of AQ method is to directly synthesize H2O2 from H2 and O2, which is environmentally friendly, simple in reaction conditions, and suitable for small-scale on-site production of H2O2[10][1]. However, there is a hidden danger that the mixture of H2 and O2 is easy to explode, and the reaction is a disproportionation reaction, which leads to a decrease in the yield of H2O2[11]. Therefore, there is an urgent need to develop more environmentally friendly, safer, and more efficient methods for the production of H2O2.
Photocatalytic production of H2O2 has attracted great attention in recent years[3]. Photocatalytic production of H2O2 is the synthesis of H2O2 from H2O and O2 by solar catalysis, which converts solar energy into chemical energy[3]. H2O and O2 are abundant and environmentally friendly raw materials on the earth, and solar energy is the cleanest and most abundant renewable energy, so photocatalytic production of H2O2 is of great significance for China to achieve the "double carbon" goal and promote the development and utilization of clean renewable energy.
In this review, recent advances in photocatalytic production of H2O2 at home and abroad are summarized, and typical catalytic systems such as graphite-like carbon nitride, metal oxides, transition metal sulfides and organic frameworks are introduced.On this basis, the shortcomings of current photocatalytic H2O2 production were analyzed, and the strategies to improve the efficiency of photocatalytic H2O2 production were discussed.Finally, the future research and application directions were prospected.

2 Mechanism of photocatalytic H2O2 production and reasons for its low selectivity

The mechanism diagram of photocatalytic H2O2 production is shown in Fig. 1: photoexcited photogenerated holes (h+) in the valence band (VB) of the catalyst undergo a four-electron water oxidation reaction (4e-WOR) to generate O2 (formula 1);H2OThe oxidation-generated O2 and adventitious O2 undergo a two-electron oxygen reduction reaction (2e-ORR) with the photogenerated electrons (e-) in the conduction band (CB) to generate H2O2 (Equation 2). Therefore, the H2O2 produced by the reaction of H2O and O2 under illumination can be expressed as Formula 3 (Formula 3).
2H2O+4h+→O2+4H+ (1.23 V vs. NHE)
O2+2e-+2H+→H2O2 (0.68 V vs. NHE)
2H2O+ O2 →2H2O2 ΔG=117 kJ·mol-1
The photocatalytic route to H2O2 depends on the type of photocatalyst and reaction conditions, and mainly includes three pathways: one-step two-electron ORR, two-step one-electron ORR, and two-channel pathway[13,14][15⇓~17][18⇓⇓⇓~22].
Tsukamoto et al. Reported a titanium dioxide (TiO2) photocatalyst loaded with gold-silver (Au-Ag) bimetallic alloy particles, which can realize 2e-ORR to generate H2O2[13]. The mechanism is that ultraviolet light excites Au-Ag/TiO2, and h+ at VB and adsorbed C2H5OH molecules undergo oxidation reaction to generate CH3CHO and proton (H+) (Formula 4); e- and adsorbed O2 molecules at the CB undergo a one-step two-electron ORR to generate H2O2 (Formula 5) (Fig. 2).
C2H5OH+2h+→CH3CHO+2H+(1.45 V vs. NHE)
2e-+O2+2H+→H2O2(0.68 V vs. NHE)
Xu et al. Reported alkali-assisted graphite-like phase carbon nitride (a-C3N4), which can realize two-step e-ORR generation of H2O2[15]. After illumination excitation, e--h+ pairs are generated on a-C3N4, and O2 is reduced by single e- to generate superoxide radicals (· O 2 -).This is followed immediately by the binding of H+ to form · H O 2 - molecules, which further react with mono e- to form H O 2 - ions. Ultimately, H O 2 - combines with H+ to generate H2O2 (Equation 6, 7, 8, 9). H+ is provided by the reaction of H + with C2H5OH (fig. 2).
O2+e-→· O 2 - (-0.18 V vs. NHE)
· O 2 -+ H+→·H O 2 -
·H O 2 -+ e-→H O 2 -
H O 2 -+H+→H2O2 (1.05 V vs. NHE)
Li et al. Reported a photocatalyst (CN1.8/ICT/CDs) loaded with 5,11-bis (4-ethynylphenyl) -5,11-indoline [2-b] carbazole (small organic molecule, ICT) and carbon quantum dots (CDs) on carbon nitride, which could generate H2O2 via a two-channel pathway[20]. ICT as the active center of ORR reduces O2 to H2O2 (formula 10), and CDs as the active center of WOR oxidizes H2O to H2O2 (formula 11) (Fig. 2).
O2+2H++2e-→H2O2(0.695 V vs. NHE)
2H2O→H2O2+2H++2e-(1.76 V vs. NHE)
At present, there are many studies on the formation pathway of photocatalytic H2O2 production, which is thermodynamically easier to carry out than photocatalytic decomposition of H2O to produce hydrogen (H2) and photocatalytic nitrogen fixation (N2). Moreover, the energy of photons in the whole visible region (380 ~ 780 nm) is enough to drive the reduction of molecular oxygen to H2O2. But in fact, under visible light (λ = 420 nm), the highest apparent quantum efficiency (AQE) of photocatalytic synthesis of H2O2 is only about 18%, which is lower than the maximum AQE (~ 30%) of decomposition of H2O to produce H2[22,77][12]. At present, the solar-to-chemical energy conversion efficiency (η, SCC) of photocatalytic H2O2 production is generally less than 1%[24].
The low efficiency of photocatalytic H2O2 production is mainly due to the small absorption range of photocatalyst for sunlight, easy recombination of e--h+, more side reactions and poor selectivity of H2O2[1,23⇓⇓⇓⇓⇓⇓⇓⇓⇓⇓ ~34]. Among them, the most critical factor affecting the efficiency of photocatalyst to produce H2O2 is the selectivity of H2O2. There are two main reasons for the low selectivity of H2O2. First of all, because of the band position of the catalyst itself, three ways of photocatalytic generation of H2O2 have been introduced above, and researchers prefer to see 2e-ORR and 2e-WOR. It can be seen from figs. 3A and 3B that the bottom potential of the conduction band of the photocatalyst meets the requirement of e-ORR, and the top potential of the valence band meets the requirement of 4e-WOR, and the 4e-ORR is easier to carry out than the 2e-ORR through density functional theory (DFT) calculation and thermodynamic analysis (fig. 3C)[35]. The second is the adsorption state of O2. There are three types of adsorption of O2 on the metal surface, one end-pair type (Pauling-type), two side-pair types (Griffiths-type and Yeager-type)[35,36]. The key to avoiding 4e-ORR is to prevent O-O bond dissociation in the adsorbed *OOH(2e-ORR the sole intermediate)[35]. The end-on adsorption of O2 can maximally reduce the O-O bond dissociation and suppress the 4e-ORR[37]. However, both end-on and side-on adsorption of O2 exist on the metal surface, so it is necessary to control the adsorption state of O2 on the catalyst surface[38].
In addition, the photocatalytic production of H2O2 involves many side reactions.Proton combines with electron to produce H2(2H++2e-→H20 V vs.NHE), e-ORR product · O 2 - is oxidized by proton to singlet oxygen (· O 2 - +h+→1O20.34 V vs.NHE), etc.The presence of these side reactions can also reduce the selectivity of photocatalytic H2O2 production[39][40]. At the same time, the decomposition reaction of H2O2 itself will lead to a decrease in the efficiency of H2O2 production. For example, :H2O2 is oxidatively decomposed by h+ (H2O2+2h+→O2+2H+,1.76V vs.NHE)[9].

3 Photocatalytic H2O2 material

At present, the typical catalyst materials for photocatalytic generation of H2O2 include g-C3N4, metal oxides, metal sulfides and organic frameworks.

3.1 Graphite-like carbon nitride

g-C3N4 is an N-type semiconductor photocatalyst of a macromolecular nonmetallic polymer, which has a superimposed two-dimensional (2D) triazine structure connected by a tertiary amine, and has a simple synthesis process and cheap and readily available raw materials[24]. Because the g-C3N4 is prepared under high temperature calcination and is composed of C-N conjugated bonds, it is difficult to destroy its structure by photogenerated carriers, resulting in the strong photocatalytic stability of the g-C3N4[28]. The band gap of g-C3N4 is about 2.7 eV, corresponding to a light absorption cutoff wavelength of 460 nm, making it a potential photocatalyst that can absorb visible light[29]. The CB bottom potential is -1.3 V vs. NHE, which is lower than the reduction potential of the V vs. NHE (-0.28 V vs. NHE), and the VB top potential is 1.4 V vs. NHE, which is lower than that of the metal oxide, thus effectively preventing the oxidation and decomposition of the V vs. NHE[1]. However, the bulk g-C3N4 photocatalyst has many disadvantages, such as fast recombination speed and slow transmission of :e--h+, low specific surface area and weak visible light harvesting ability[30][31][32][33]. Table 1 summarizes the activity of the g-C3N4 photocatalytic system to produce H2O2 (where the ratio of sacrificial agent to H2O is the volume ratio, AQY is the apparent quantum yield, and Tables 2, 3, and 4 are the same).

3.2 Metal oxide

Metal oxides have the advantages of low cost, relatively good stability and biocompatibility, easy preparation and various modification strategies[34]. In addition, appropriate band positions endow metal oxides with good reduction and oxidation abilities, which are favorable for ORR and WOR[34]. Therefore, metal oxide photocatalyst is a good substitute for organic semiconductor g-C3N4. Currently, metal oxide photocatalysts developed and used to produce H2O2 mainly include titanium dioxide (TiO2), tungsten trioxide (WO3), zinc oxide (ZnO), and bismuth vanadate (BiVO4).
In 1972, Japanese scientists Fujishima and Honda reported that TiO2 as anode materials could decompose water under ultraviolet irradiation, which opened up the research of semiconductor TiO2[41]. In addition, its CB bottom potential (0.19 V vs. NHE) is more negative than the two-electron reduction potential of V vs. NHE (0.68 V vs. NHE), which favors the photocatalytic generation of V vs. NHE[1]. The H2O2 generated by ZnO photocatalysis is not easy to be adsorbed on the surface of ZnO, so ZnO can inhibit the decomposition of H2O2[42]. However, TiO2 and ZnO have common disadvantages: firstly, their band gaps are too large (about 3.2 eV and 3.37 eV, respectively), resulting in extremely low solar utilization efficiency[43,44]; Secondly, it is easy to be corroded by light in the reaction system, Ti-OH on the surface of TiO2 is easy to form peroxide Ti-OOH, and ZnO is easy to be oxidized by h+[9][45]. All of these disadvantages can lead to the decrease of the selectivity of the photocatalyst to produce H2O2. However, the band gaps of WO3 and BiVO4 are relatively small (2.6 eV and 2.4 eV, respectively), and the absorption range can be extended to the visible range[46,47]. However, pure WO3 and BiVO4 are excited by light to produce e--h+ pairs, which are easy to recombine and lack ORR active sites, resulting in almost no content of H2O2 produced by their photocatalysis[46,48]. The photocatalytic activity of metal oxide materials for H2O2 production is summarized in Table 2.

3.3 Metal sulfide

Metal sulfides (ZnS, CdS, Zr2S3, and In2S3, etc.) generally have higher CB sites and wider photoresponse range than metal oxides[23]. However, they have poor adsorption capacity for reactants and poor photostability, which lead to an increase in the recombination rate of photogenerated charges, so they need to be further modified for efficient photocatalytic production of H2O2. Adjusting the proportion of metal ions in the precursor to construct multi-metal sulfide semiconductor catalysts is a common technical means at present. For example, adjusting the molar ratio of indium ion (In3+) and gallium ion (Ga3+) in CuInxGa1-xS2, its band gap has a linear relationship with the molar ratio of In3+ and Ga3+[49]. As such,The In3+ in the In2S3 is made of Cu+,Plasma replacement of Ag+, Zn2+ and Cd2+,Heterogeneous photocatalysts are further constructed to meet the energy level requirements and adsorption requirements of various photocatalytic reactions[50⇓⇓⇓~54]. Table 3 summarizes the activity of metal sulfide material photocatalytic system for H2O2 production.

3.4 Organic framework

Organic frameworks include covalent organic frameworks (COFs) and metal-organic frameworks (MOFs). COFs are crystalline microporous materials assembled by organic molecules through strong covalent bonds in a network synthesis process, so COFs have high porosity, strong thermal and chemical stability[60⇓~62]. MOFs are a kind of high porosity crystalline materials designed and synthesized by using metal ions and organic ligands. MOFs are considered to be excellent candidates for photocatalysts because of their unique coordination connection, which can select different metal centers and organic ligands for pairing, tunable structure and strong gas adsorption ability[63]. But COFs and MOFs catalysts also suffer from the defects of easy recombination of e--h+ pairs and lack of ORR active sites. Table 4 summarizes the activity of the organic framework photocatalytic system for H2O2 production.

4 Modification Strategy of Photocatalyst Material

Generally, high catalytic activity of photocatalyst requires the following conditions: appropriate band gap, visible light absorption, effective generation, high-speed transfer and recombination rate of photogenerated carriers, and more reactive sites[61]. From the previous analysis, it can be seen that the efficiency of photocatalytic H2O2 production is low, and improving the efficiency of photocatalytic H2O2 production is the key to whether photocatalytic H2O2 can be applied to industry. Morphology control, defect engineering, heterojunction engineering, modification of organic molecules or groups and quantum dots, loading of metal nanoparticles, element doping and construction of three-phase reaction system are the main strategies to improve photocatalysis to produce H2O2, among which defect engineering is mainly aimed at the modification of g-C3N4.

4.1 Morphology control

Morphology optimization is a feasible method to modify the physicochemical properties of g-C3N4, with the main purpose of increasing its specific surface area and providing more active sites for the reaction[64]. Since the specific surface area of the original g-C3N4 is small, only about 10 m2/g, the g-C3N4 can be designed into structures such as hollow microspheres, ultrathin nanosheets, tubes and layered tubes to improve its specific surface area and increase reactive active sites[27][26,66][68,69][24,70]. For example, Lu et al. Reported g-C3N4(PT-g-C3N4) modified by dielectric barrier discharge (DBD) plasma[71]. Compared with the original g-C3N4, the crystal size of the PT-g-C3N4 is reduced from 99. 2 nm to 57. 2 nm, and the specific surface area and pore volume are increased by 15% and 33. 8%, respectively. The results showed that after 60 min of reaction, the concentration of H2O2 produced by PT-g-C3N4 photocatalysis was 14. 46 μmol/L, which was 13 times higher than that of the original g-C3N4. This can be attributed to the enlarged specific surface area of PT-g-C3N4, which leads to the increase of surface active sites and promotes the generation of H2O2.
The tubular structure of g-C3N4 is considered to be the ideal morphology, but the wall of tubular g-C3N4 is too thick to facilitate the electron migration from the interior to the surface, thus inhibiting the separation of photogenerated carriers[24]. Yu et al. Prepared 3D layered tubular g-C3N4(NCNT-25) with uniform diameter under 25 mL/min of N2 atmosphere[70]. The specific surface area of NCNT-25 is 96.11 m2·g-1, which is more than 13 times that of BCN. In the O2/ ethanol (EtOH)/H2O system, the H2O2 formation rate is 485.7μmol·h-1·g-1, which can be attributed to the fact that the multilayer nanotube 3D network significantly expands the optical absorption range of the catalyst, enhances the mass transfer rate and suppresses the e--h+ pair recombination.
Morphology optimization will also be applied to other catalyst materials. For example, the columnar precursor of In2S3 prepared by MOF method can effectively increase its porosity and specific surface area[53,72]. Similarly, with the increase of the content of the Ti3C2 in the precursor solution, a TiO2 is formed on the surface of the Ti-based MOF(NH2-MIL-125), and the TiO2 changes from two-dimensional nanosheets to three-dimensional nanoparticles, which can accelerate the separation and transfer of e--h+[75]. In addition, the spherical shape of the TiO2 colloid is beneficial to the deposition of Au nanoparticles with monodisperse size[76]. Changing the crystalline phase of the catalyst is also a means to change the morphology. For example, the tetragonal phase BiVO4 is converted to the monoclinic phase BiVO4 through hydrothermal treatment, and the (010) and (110) of the monoclinic phase BiVO4 are further loaded with co-catalysts, thereby solving the problem that the photocatalysis of the tetragonal phase BIVO4 generates almost negligible H2O2[73,74]

4.2 Defect Engineering

Controlled carbon/nitrogen vacancies in g-C3N4 can be easily created by changing the S-triazine unit of g-C3N4 without destroying the whole structure (Fig. 4)[79]. The methods of vacancy formation include heat treatment, chemical treatment, microwave-assisted treatment, etc[79].

4.2.1 C vacancy

The generation of C vacancy will reduce the symmetry of g-C3N4 and produce electron delocalization effect, which will make g-C3N4 have more excitable electrons and narrower band gap. On the other hand, carbon vacancies provide more sites to adsorb molecular O2[80].
Xie et al. Reported that a mixture of melamine-cyanuric acid (MCA) supramolecular aggregates and oxalic acid was heated by microwave for 7 min to obtain oxygen-doped g-C3N4(O-CNC) containing C vacancies[81]. The synthesized O-CNC has large specific surface area and mesoporous structure. The synergetic effect of C vacancy and O doping optimizes the charge separation, harmonizes the energy band structure, and significantly promotes the formation of H2O2 from 2e-ORR. Under simulated solar irradiation, the photocatalytic generation rate of H2O2 is 2008.4μmol·h-1·g-1, which is more than four times the efficiency of pristine bulk CN.
Lei et al. Introduced the inverse opal (IO) structure and carbon vacancy (Cv) into the g-C3N4(IO-CN-Cv) to improve the efficiency of photocatalytic H2O2 generation[82]. With EtOH as sacrificial reagent, IO-CN-Cv catalyzed the formation of 325.74μmol·L-1 of H2O2 without EtOH as 46.26μmol·L-1 after 2 H of visible light irradiation. This again verified that the presence of alcohols as sacrificial agents would promote the formation of H2O2, because h+ would preferentially react with EtOH to promote the formation of H+[136].

4.2.2 N vacancy

The presence of N vacancies in the tri-S-triazine repeating unit of g-C3N4 leads to the narrowing of the intrinsic band gap and the formation of in-gap defect States, thereby expanding the visible light absorption range and suppressing the e--h+ pair recombination[83]. In addition, N vacancies create a large number of unsaturated sites and induce interlayer interactions, resulting in highly efficient excitation of electrons and facilitating charge transport[84].
Liu et al. Reported the synthesis of bulk g-C3N4 by thermal polymerization, followed by gradient calcination (2.5℃·min-1) of bulk g-C3N4 to prepare g-C3N4 ultrathin nanosheets (CNS),The CNS powder was next gradient-calcined (2.5℃·min-1) under N2 atmosphere to introduce N vacancies (Fig. 5)[26]. The advantage of this method is that a single type of defect can be introduce accurately and with a controlled concentration in that framework of the g-C3N4. Multi-step calcination increases the specific surface area of g-C3N4, which provides more O2 adsorption and active sites for the reaction. As the defect level increases, the band gap of the g-C3N4 gradually narrows, thereby increasing the visible light absorption range, accelerating the charge transfer and improving the separation efficiency of photogenerated carriers. The best sample CNS-500 produced a 498μmol·L-1 H2O2 within 30 min, which was 18 times higher than that of pure CN. The AQE was estimated to be 4.41% (λ = 420 ± 10 nm), which is 25 times higher than that of pure CN.
Zhang et al. Reported that cyano group (— C ≡ N) and N vacancy were introduced into g-C3N4(Nv—C≡N—CN) in turn, and the preparation process is shown in Fig. 6a: firstly, thiourea was added into urea, and — C ≡ N modified g-C3N4(C≡N—CN) was generated by thermal polymerization in a fully closed crucible[86]; Subsequently, hot etching was carried out in Ar atmosphere to introduce N vacancies (Nv — C ≡ N — CN). The changes of molecular structure and micromorphology (scanning electron microscopy (SEM)) are shown in Fig. 6 B and C. With IPA as sacrificial reagent, the formation rate of ( λ ≥ 420 nm),H2O2 reached 3090 mmol·g-1·h-1 under visible light irradiation, and the AQE at 400 nm reached 36.2% with SCC efficiency of 0.23%. This is because Nv — C ≡ N — CN has a larger specific surface area and more pores (Figure 6C), and this microstructure helps to expose more active sites and increase the contact area with O2. In addition, the mechanism of double defects is clear: — C ≡ N can promote the adsorption of H+, and N vacancy can promote the adsorption of O2. The synergistic effect not only improves the visible light absorption ability (the band gap of Nv — C ≡ N — CN is reduced from 2. 43 eV to 1. 88 eV), but also improves the carrier separation ability, and promotes the conversion of intermediate ·HO2- to H2O2.

4.2.3 Other defects

C/N vacancy is a unique modification method of g-C3N4, in addition, there are some other defects reported. Tian et al. Reported that zirconium trisulfide nanobelts (ZrS3NBs) with S 2 2 - and S2- vacancies could photocatalytically generate H2O2 with high efficiency[87]. Electron paramagnetic resonance (EPR) spectrum shows that ZrS1-yS2-x(15/100)NBs is located at the characteristic peak at G = 2.0075, indicating the formation of S2- and S 2 2 - vacancies. After a systematic study of the effect of S 2 2 - and S2- vacancies on carrier dynamics and photocatalytic performance,It is found that the S 2 2 - vacancy can significantly promote the separation of photogenerated carriers, while the S2- vacancy promotes the transfer of e- and h+. In addition, the ZrS1-yS2-x(15/100)NBs photocurrent increases, indicating that the S 2 2 - and S2- vacancies are able to extend the "lifetime" of carriers. Chen et al. Reported an advanced photocatalyst (In2S3@Ov/In2O3) for the generation of oxygen vacancies (Ov) by Ar plasma treatment of tubular In2O3 followed by the growth of In2S3 nanoflowers[88]. The Ov active sites on the composite can capture e-, which promotes the separation of e--h+ pairs of the photocatalyst. In addition, Ov may adjust the H2O2 generation route from one-electron ORR to two-electron ORR. Moreover, the porous In2S3@Ov/In2O3 composite has a considerable light absorption edge and a strong "light trapping" microstructure, which significantly improves its utilization of visible light. The achieved data showed that the photocatalytic H2O2 generation rate of In2S3@Ov/In2O3 in pure water was 4.59μmol·g-1·min-1, and the AQY at 420 nm was 28.9%.
Defect engineering of MOFs is a promising approach that can tune the electronic structure, surface chemistry, and porosity of MOFs[89]. Kondo et al. Synthesized UiO-66-NH2 from zirconium tetrachloride (ZrCl4) and 2-aminoterephthalic acid by solvothermal method, and used acetic acid as a regulator for defect introduction[90]. With the increase of acetic acid concentration, the number of defective linkers increases, which will improve the hydrophobicity of the UiO-66-NH2. The rapid separation of H2O2 and catalyst can inhibit the decomposition of H2O2, and also promote the charge transfer process from linkers to clusters, resulting in the consumption of carriers.

4.3 Heterojunction engineering

Heterojunction photocatalyst can effectively enhance the separation of photogenerated carriers, so the appropriate design of heterojunction in photocatalyst can effectively improve its photocatalytic activity[91]. At present, the most studied heterojunctions are Z-type heterojunction (Fig. 7A) and S-type heterojunction (Fig. 7B). Z-type heterojunction, commonly known as PN junction, was first proposed by Bard in 1979[92]. The principle of photocatalysis is that h+ in VB of PS I reacts with electron donor (D) to produce the corresponding electron acceptor (A), and conversely, e- in CB of PS II reacts with A to produce D; Then, e- retained in the CB of PS I and h+ in the VB of PS II participate in the reduction and oxidation reactions, respectively[93]. The S-type heterojunction is mainly composed of two N-type semiconductors (NN junction), representing an oxidizing photocatalyst (OP) with a larger work function and lower Fermi level and a reducing photocatalyst (RP) with a smaller work function and higher Fermi level[94]. Under the irradiation of light, both semiconductor materials are excited, and electrons jump from the valence band (VB) to the conduction band (CB), unlike the Z-type heterojunction, the more active e- and h+ are retained in the CB of RP and the VB of OP, respectively, while the useless photogenerated carriers are recombined, and the e--h+ pair is effectively separated in space, so that it can obtain stronger redox ability[95].

4.3.1 Z-heterojunction

Our research group reported the Lu3NbO7:Yb,Ho/CQDs/AgInS2/In2S3Z--type heterojunction photocatalyst, and the preparation process is shown in Fig. 8C[72]. The photocurrent diagram (Fig. 8 a) and electrochemical impedance spectroscopy (EIS, Fig. 8 B) illustrate that the e--h+ pair has good photoresponse ability and separation efficiency. This may be due to the fact that CQDs, as an electron conducting medium, significantly enhanced the visible light absorption and electron transfer rate of the heterogeneous pair, and the concentration of H2O2 was 902. 9 μmol/L after 5 H. Chen et al. Reported the preparation of ultrathin g-C3N4 nanosheets by two-step gradient calcination (30 ° C/min) of melamine precursor — as a support for carbon quantum dots (CQDs) to construct a Z-type heterojunction photocatalyst (α-Fe2O3/CQD@g-C3N4) with α-Fe2O3[96]. The ultraviolet-visible diffuse reflection absorption (UV-vis DRS) spectrum shows that the α-Fe2O3/CQD@g-C3N4 can absorb visible light of nearly 800 nm, while the absorption edge of the ultrathin g-C3N4 is only 441 nm (Fig. 9d), because CQDs are used to compensate for the shortcomings of the ultrathin g-C3N4 in terms of wide band gap. Moreover, the exposed α-Fe2O3 changes the pathway of α-Fe2O3/CQD@g-C3N4 catalysis to H2O2, optimizing from one-electron ORR to two-electron ORR.
Zhang et al. Used a simulation method to synthesize multilayer SnS2/MoO3 hollow nanotubes[97]. 3D SnS2/MoO3 exhibits higher charge transfer ability due to its hollow structure and high specific surface area (55.8 m2·g-1, which is 1.96 and 4.36 times that of SnS2 and MnO3, respectively), and also provides more active centers. Zheng et al. Reported a single-component NH2-MIL-125 photocatalyst with coexisting (111) and (001) faces, which can photocatalytically generate H2O2 through a two-channel pathway[98]. One channel is the reduction of O2 by e- at CB on the (111) face, and the other channel is the oxidation of OH- by h+ at VB on the (001) face. This Z-type heterojunction structure accelerates the space charge separation, and the H2O2 yield reaches 917μmol·g-1·h-1 in pure water system, which is 1.30 and 1.14 times higher than that of MIL-001 and MIL-111, respectively.

4.3.2 S-type heterojunction

Using ZIF-8 and urea as precursors, Liu et al. Prepared S-type heterojunction photocatalyst (ZCNx: X is the weight/G of urea in the precursor) of layered porous ZnO/g-C3N4 by two-step calcination method[99]. EPR analysis shows that the photoinduced e- and h+ are distributed in the CB of CN and the VB of ZnO, respectively, which is a typical S-type heterojunction scheme. Due to the effective separation of the e--h+ of ZCN12 and the enhancement of the · O 2 - signal, the concentration of H2O2 generated by ZCN12 in 1 H was 1544 μmol/L, which was 5.0 and 3.4 times higher than that of pure ZnO and pure CN, respectively (Fig. 9 A). However, the S-type heterojunction promotes the generation of H2O2 as well as the decomposition of H2O2 (Fig. 9b), so promoting the generation of H2O2 while inhibiting the decomposition of H2O2 has been the focus and difficulty of people's research.
Li et al. Reported a tungsten oxide (S-pCN/WO2.72)S--type heterojunction photocatalyst with S-doped porous g-C3N4 and oxygen vacancies on the surface[100]. In the heterojunction formation process, the electronic defect of oxygen vacancy on the surface of WO2.72 can be filled by the lone pair electrons of sulfur and nitrogen elements on S-pCN. By adjusting the recombination ratio, suitable oxygen vacancies are generated on the WO2.72 surface, which promotes electron transfer and radical generation. The internal electric field (IEF) and band bending effect accelerate the transfer of photogenerated charges on the interface, thereby promoting the recombination of unwanted photogenerated carriers, retaining e- and h+ with high redox potential, and improving the separation and utilization efficiency of photogenerated carriers. Similarly, Yang et al. Reported that TiO2 nanofibers were prepared by electrospinning, and In2S3 nanosheets were grown in situ on their surface, which successfully constructed TiO2/In2S3S--type heterojunction photocatalyst[101]. Driven by the IEF, band-bending effect and Coulomb interaction, the carriers (e- in the CB of TiO2 and h+ in the VB of In2S3), which are considered to be "useless", will spontaneously recombine. In contrast, the recombination of electrons in the CB of In2S3 and holes in the VB of TiO2 is suppressed, and these "useful" carriers with higher oxidation and reduction abilities are preserved in the CB of In2S3 and the VB of TiO2, respectively.
Wang et al. Reported a Cu2(OH)PO4/g-C3N4S--type heterojunction photocatalyst that can respond to the full spectrum[19]. CN/CuPO (20 wt%) shows obvious O2-TPD signals in the temperature range of 400 – 560 ° C (Fig. 9c), indicating that the O2 adsorption capacity of the composite catalyst can be significantly improved after coupling of CN with Cu2(OH)PO4. As the adsorbed O2 molecules will consume e-, the separation efficiency of e--h+ pair will be improved, and it is proved that this is because of the effect of P O 4 3 - ions produced after coupling. Zhao et al. Reported a g-C3N4 assisted Ni-CAT composite catalyst, which can realize double 2e-ORR to produce H2O2[102]. Ni-CAT has a large specific surface area and abundant mesoporous structure, which is the main active carrier and oxygen-rich center for ORR[103]. The role of g-C3N4 is to suppress the carrier recombination of Ni-CAT by donating electrons. Chen et al. Modified the organic semiconductor perylenetetracarboxylic diimide (PDI) on the MIL-125-NH2 to construct an S-type heterojunction structure (MIL-125-PDI), which promoted the separation and transfer of photogenerated charges[104]. Under visible light irradiation (λ > 420 nm), the photocatalytic generation rate of H2O2 by MIL-125-PDI was 4800μmol·g-1·h-1, which was 4.3 times higher than that of MIL-125-NH2.

4.4 Supported metal nanoparticles

Metal nanoparticles (NPs) with catalytic activity are loaded on the photocatalyst, and a Schottky barrier is formed at the interface between the noble metal and the semiconductor, which can promote charge separation and improve the photocatalytic activity[34][105].
Jiang et al. Synthesized in situ graphene-like g-C3N4 supported interfacial plasmonic gold nanoparticles (Au NPs) photocatalyst without physical barrier (Au/C3N4) from a homogeneous mixture of HAuCl4 and urea by one-step polymerization[106]. The loading of Au NPs enhanced the visible light harvesting ability of Au/C3N4 and promoted the directional transfer of e- from the N 2p orbital of C3-N species in g-C3N4 to Au during photocatalysis. Therefore, Au/C3N4 photocatalysis has a high selectivity to generate active species such as · OH, · O 2 -, and H2O2. Cai et al. Prepared Ag NPs supported ultrathin g-C3N4 nanosheet photocatalyst (Ag@U-g-C3N4-NS)[107]. The improvement of the photocatalytic performance of Ag@U-g-C3N4-NS is mainly attributed to the following reasons: Ag NPs induce the surface plasmon resonance (SPR) effect of Ag@U-g-C3N4-NS, which increases the absorption range of the photocatalyst for visible light; Ag NPs and U-g-C3N4-NS form a Schottky barrier to suppress photogenerated charge recombination.
Meng et al. Used Au NPs supported ZnO for efficient photocatalytic generation of H2O2(1.5 mmol·L-1·h-1)[108]. Because the high selectivity of Au NPs for 2e-ORR and the ZnO inert surface inhibit the decomposition of H2O2. Wang et al. Reported that Au NPs deposited WO3 was used for efficient photocatalytic generation of H2O2[109]. 0.5 wt% Au NPs were deposited and could catalyze the formation of 576 μmol of H2O2 within 400-Au0.5/WO3,5 h of the sample calcined at a high temperature of 400 ° C.
Liu et al. Reported a molybdenum-doped BiVO4(Mo:BiVO4) system with precise loading of CoOx and Pd on the Mo:BiVO4(110) plane and (010) plane, respectively (Fig. 10 a)[74]. Fig. 10 B, C and d are SEM diagrams during loading, respectively. Fig. 10c shows that the CoOx particles are uniformly distributed on the (110) plane of Mo:BiVO4. The energy dispersive X-ray spectroscopy (EDS) elemental map (Fig. 10e) and spectral map (Fig. 10f) are also verified, and the CoOx signal on the (110) plane is 4.1 times stronger than that on the (010) plane. Loading the co-catalyst on different faces can tailor the interfacial energy between the (110) and (010) faces while promoting charge separation in Mo:BiVO4. In the absence of sacrificial agent, the H2O2 yield was 1425μmol·h-1 and the AQY at 420 nm was 5.8%.
Chen et al. Reported the deposition of NiO NPs and Pt NPs on MIL-125-NH2 using Ni(NO3)2·6H2O and H2PtCl6 as metal sources, respectively, and hydrazine hydrate as a reducing agent[110]. It was found that NiO/MIL-125-NH2 significantly increased the amount of H2O2 formation, but not because of the increase in the formation rate, but because NiO inhibited the decomposition of H2O2. Kim et al. Reported a solid-phase porous TiO2 film loaded with Au nanodomain photocatalyst (Au NIs/TiO2), which could generate millimolar level H2O2 in 5 min, 80 times that of pure TiO2 film[111]. This is mainly attributed to the fact that the porous structure of the :TiO2 film can effectively scatter UV light, thereby increasing the generation of e--h+ pairs in the TiO2; Au loading generates area planes of various sizes on the surface of the TiO2, a potential gradient can be formed through the small Au area plane, the TiO2 and the large Au area plane, the Schottky barrier at the junction of the small Au area plane /TiO2 is reduced, and the recombination of photogenerated electron-hole pairs is inhibited[13]. In addition, Moon et al. Reported that rGO acted as a co-catalyst for TiO2, and the catalytic activity was comparable to that of noble metals (Au, Ag, and Pt) supported on TiO2[112]. And the addition of phosphate to the rGO/TiO2 for in situ growth of the CoPi complex can effectively promote the generation of H2O2.

4.5 Element doping

Doping elements can effectively adjust the electronic structure of photocatalyst and broaden its visible light absorption range[34]. Element doping strategies are mostly prepared by calcination of the precursor in one step, the regulation of metal sites can improve the activity and selectivity of ORR, and the regulation of non-metal sites may lead to higher local electron density, which enhances the activity of photocatalytic H2O2 production[37][113].

4.5.1 Metal element doping

Teng et al. Reported the preparation of a robust Sb single-atom photocatalyst (Sb-SAPC, single Sb atom dispersed on g-C3N4) by wet chemical method using NaSbF6 and melamine as precursors[37]. O2 is adsorbed on the separated Sb atomic sites, which promotes the formation of Sb-OOH and thus promotes the production of H2O2 from 2e-ORR. At the same time, the holes accumulated on the N atoms near the bulk unit of the Sb site kinetically accelerate the oxidation of H2O. Under visible light irradiation, the optimal sample formation H2O2 rate was 17. 6% (420 nm) for 12.4 mg·L-1(2 h),AQE and 0. 61% for SCC efficiency. Moscow et al. Synthesized efficient BiVO4 nanocatalysts doped with erbium (Er) and yttrium (Y) through a simple microwave irradiation route[134]. Through the formation of internal energy States of rare earth metal, the band gap of BiVO4 is greatly reduced, the optical absorption ability is enlarged, and the recombination rate of photoexcited e--h+ pairs is reduced.

4.5.2 Non-metallic element doping

Liu et al. Effectively improved the photocatalytic activity of g-C3N4 for H2O2 generation by using the synergistic method of element doping and morphology regulation[114]. Melamine and cyanuric acid were used to prepare MCS crystals by hydrothermal synthesis, and then CNT was synthesized by thermal polymerization. CTN was used to synthesize B-CNT, P-CNT and S-CNT photocatalysts by thermal polymerization with boric acid, ammonium dihydrogen phosphate and thiourea, respectively (Fig. 11). The H2O2 generation rates catalyzed by B-CNT, P-CNT, and S-CNT are 42.31μmol·min-1, 24.95μmol·min-1, and 24.22μmol·min-1, respectively, which are higher than the 16.40μmol·min-1 of bulk BCN. This is because the tubular CN with special structure enhances the light-harvesting ability through the multiple reflection effect, and the doping of B, P and S atoms can adjust the electronic structure of CNT, which helps to improve the separation efficiency of photogenerated carriers. In addition, Xu et al. Also reported that C doping could effectively shorten the band gap of g-C3N4, thereby broadening the optical absorption range and enhancing the reduction ability of e-[115].
Feng et al. Reported the doping of S element (SS-CN) in g-C3N4 nanosheets, and the introduction of S in the heptazine unit could adjust the band structure and local charge density of g-C3N4[113]. SS-CN greatly promotes light absorption, charge separation, carrier density (8.7-fold increase), and surface charge transfer efficiency. Under the irradiation of visible light, the H2O2 generation efficiency was 566.69μmol·g-1·h-1. Hirakawa et al. Found that under visible light irradiation, TiO2 doped with N and S can produce · O 2 -, which can not be observed on TiO2 under the same conditions[116]. Moreover, the S-doped TiO2 is superior to the N-doped TiO2 in the ability to generate a O 2 -.While N-doped TiO2 outperformed S-doped TiO2 in accumulating H2O2. Lee et al. Prepared CdS NPs by using Cd(EDDA)(EDDA2-=2,2'- (ethylenedithio) diacetate) as the precursor of MOFs, and combined them with heteroatom-doped carbonaceous supports to form nanocomposite photocatalysts[117]. Cd (EDDA) is an ordered crystalline solid consisting of coordination bonds between Cd (Ⅱ) ions and S based organic ligands. After simple annealing, it was transformed into a composite, in which S and C were uniformly distributed around the 5 nm sized CdS NPs. Due to the hydrophobicity of H2O2, the presence of S and C can prevent the adsorption of H2O2, thereby inhibiting the decomposition of H2O2.

4.6 Quantum dot modification

Quantum dots have been rapidly developed as active centers for photocatalysis because they facilitate fast charge transfer and have excellent e- trapping ability[118]. In addition, quantum dots can also broaden the absorption edge of some catalysts to the visible light range, and significantly inhibit the decomposition of H2O2, while promoting selective 2 e-ORR, thereby increasing the yield of H2O2.
Yang et al. Reported metal-free heterostructured photocatalysts (BU-X, X is the addition volume of BN QDs solution, X = 0.5, 1, 3, 5 mL) composed of boron nitride quantum dots (BN QDs) modified ultrathin porous g-C3N4(UPCN)[119]. The photoluminescence (PL) spectra show (Figure 12 a) that the emission peak intensity of UPCN and BU samples is clearly reduced compared to CN, with BU-3 having the lowest emission peak (465 nm). The significant decrease in the emission peak intensity indicates a clear reduction in the number of excitons because the photoluminescence phenomenon originates from the recombination of singlet excitons. It can be inferred that BU-3 photocatalyst can improve the dissociation efficiency of excitons and suppress the recombination of carriers by using ultrathin porous nanostructures and BN QDs. In addition, the time-resolved photoluminescence (TRPL) spectrum shows (Figure 12b) that the τ a v e of CN is 9.05 ns, while those of UPCN and BU-3 are 8.33 and 7.09 ns, respectively. The singlet exciton lifetime is significantly shortened, which obviously indicates that the dissociation of excitons in BU-3 is promoted.
Zheng et al. Reported a TiO2(SN-GQD/TiO2) modified by sulfur and nitrogen co-doped graphene quantum dots for efficient photocatalytic synthesis of H2O2[120]. SN-GQD is uniformly dispersed on the surface of TiO2, which leads to the acceleration of e- migration and the red shift of absorption edge from 400 nm to 620 nm in the visible region. In addition, GQD may provide an active site for the ORR intermediate * OOH. The experimental data showed that SN-GQD/TiO2 photocatalyzed the formation of 451 μmol of H2O2 in 1 H, which was 3. 2 times higher than that of pure TiO2. Wang et al. Reported that cadmium selenide quantum dots (CdSe QDs) modified TiO2 was used to degrade malachite green (MG), but found that H2O2 and · O 2 - were important intermediate species in the photocatalytic reaction[121]. When benzoquinone (BQ) was added to the reaction system, it was found that the degradation of MG was seriously inhibited, which indicated that O 2 - played an important role in the catalytic degradation process and was formed in large quantities during the reaction. The H2O2 in the photocatalytic process was detected by DOD method, and it was found that the CdSe QDs-TiO2 had obvious absorption peaks at 510 nm and 551 nm, while it could not be observed on the TiO2 under the same conditions, which indicated that the H2O2 was actually produced by the modification of TiO2 by CdSe QDs. Similarly, Li et al. Synthesized carbon quantum dots TiO2 nanosheets (CDs-TNs) by hydrothermal method, and found that CDs could promote the formation of H2O2 by reducing Cr (Ⅵ) under illumination[122].

4.7 Introduction of organic molecules or groups

The introduction of organic molecules or groups on the surface of g-C3N4 realizes the effective adsorption and activation of O2 molecules, inhibits the recombination of photogenerated carriers, and can dynamically improve the production efficiency of H2O2. For example, Zeng et al. Reported that polyethyleneimine (PEI) molecules were introduced to the surface of g-C3N4 to construct PEI/C3N4 nanocomposites to promote the photocatalytic generation of H2O2[123]. Because PEI molecules contain abundant amine groups, positively charged PEI can be adsorbed on the surface of negatively charged C3N4 through electrostatic attraction. Due to the electronic interaction between PEI molecules and C3N4, h+ would be captured by PEI molecules and then transported to the surface of PEI/C3N4 to react with · O 2 - molecules, which apparently inhibits the recombination of photogenerated carriers.
Yu et al. Reported a co-monomer doping strategy to tune the electronic structure of CTFs nanoshells by introducing strong electron-withdrawing benzothiadiazole units into the conjugated network, in order to tune the electronic structure of CTFs and suppress the recombination of charge carriers[25]. Multiple spectral analysis proved that the charge separation ability of CTF-NS-5BT was greatly enhanced, and the photocatalytic generation rate of H2O2 in pure water system reached 1630μmol·g-1·h-1, which was more than three times higher than that without regulation. Chen et al. Reported the introduction of acetylene or diacetylene into CTFs to generate H2O2 via 2e-ORR and 2e-WOR (Fig. 13)[125]. Compared with CTF-BPDCN, the photoluminescence intensity of CTF-BDDBN and CTF-EDDBN decreases, indicating that the photocarrier recombination in CTFs is substantially suppressed after the addition of acetylene or diacetylene. At the same time, acetylene or diacetylene moieties can change the electronic structure of CTFs and provide active sites for 2e-ORR to reduce the energy barrier formed by H2O2.
Based on the structural and functional tunability of MOFs, Li et al. Reported that 4-carboxyphenylboronic acid (CPBA) was used as a boron-containing organic ligand to replace terephthalic acid (PTA) in UiO-66, and a boron-containing zirconium-based MOFs photocatalyst (UiO-66-B) (Fig. 14a) was prepared for efficient photocatalytic generation of H2O2[126]. According to the analysis of electron density distribution (Fig. 14 B, C): for UIO-66,O2 adsorbed at the carbon site of the benzene ring; While for UIO-66-B,O2 is located at the boron site. It shows that the introduction of boron effectively utilizes the delocalized π electrons in the benzene ring to convert the electron-deficient boron into electron-donating sites, which makes UiO-66-B more conducive to the activation of O2 molecules. The calculated adsorption energy further verifies this conclusion, and the adsorption energy of O2 on UiO-66-B is − 0.81 eV, much higher than that of UiO-66 (− 0.24 eV). In addition, the stronger O2 adsorption capacity of UiO-66-B contributes to the accumulation of O2 on its surface and the generation of more · O 2 -. Compared with UiO-66, the EIS spectrum of UiO-66-B shows a smaller arc radius, which indicates that UiO-66-B has a smaller charge transfer resistance, so the carrier transfer and separation efficiency of UiO66-B is higher. Chen et al. Reported that 4,4 ′, 4 ″, 4- (pyrene-1,3,6,8-tetraacyl) tetrabenzoic acid (L2) was introduced into MIL-125 to successfully prepare MIL-125-xL2 photocatalyst (X is the amount of substance of L2 (mmol))[127]. The best sample MIL-125-0.14 L2 catalyzed the formation of H2O2 with a rate of 1654μmol·L-1·h-1. This can be attributed to the fact that the PL of MIL-125-0.14L2 is significantly reduced compared with bare L2 and MIL-125, illustrating the very efficient transfer of electrons from L2 to Ti-O clusters, which is a prerequisite for improved photocatalytic performance; The introduction of L2 caused the morphology of MOFs to change from flat to octahedral, which endowed MOFs with more structural defects of missing ligands and made their specific surface area and pore size slightly larger.

4.8 Construction of three-phase reaction system

Ligand engineering can directly affect the physicochemical properties of the catalyst, inhibiting the occurrence of side reactions through the unique steric environment and the electronic structure of the catalytic active center[88]. Based on the principle of ligand and interface engineering, considering the hydrophobicity of photocatalyst, a solid (photocatalyst) -liquid (H2O)- gas (O2) three-phase reaction system can be constructed on the premise of ensuring the function of liquid phase. Because the diffusion coefficient of oxygen in air (2×10-1cm-2·s-1) is 4 orders of magnitude higher than that in water (2.1×10-5cm-2·s-1), the diffusion of O2 molecules consumed on the catalyst surface from air to the three-phase system is more efficient compared to the two-phase system[131].
Sun et al. Reported a superhydrophobic Pd/A/BiVO4 photocatalyst with Pd supported on 3-aminopropyltrimethoxysilane (APTMS) modified BiVO4[129]. Among them, Pd is the O2 adsorption and catalytic active center, and APTMS is the bridge ligand between BiVO4 and Pd. Because of the charge transfer of the APTMS electron donor amino (-NH2) moiety, the charge density of the Pd metal center increases, resulting in higher two-electron oxygen reduction activity[130]. Moreover, -NH2 is shielded by Pd, and the hydrophobicity of Pd/A/BiVO4 is controlled by the long C — H chains of the APTMS framework. During the reaction, O2 not only acts as a substrate but also participates in the construction of the PdOx intermediate, which is determined to be the true catalytic center. Due to the above advantages, the rate of H2O2 generation in pure H2O under visible light irradiation through the two-channel pathway was 805.9μmol·g-1·h-1, and the catalyst also showed good stability in the cycling test.
Li et al. Reported that triphenylbenzene-dimethoxyterephthalic acid-COF (TPB-DMTP-COF) could efficiently photocatalyze the generation of H2O2 under visible light irradiation[131]. The prepared TPB-DMTP-COF was immobilized on porous carbon fiber paper, and a three-phase reaction system was constructed by using the hydrophobicity of this polymer semiconductor. The specific surface area of TPB-DMTP-COF was calculated as 2747 m2·g-1, and the evaluated pore size was 2.4 nm. The large specific surface area is associated with the layered structure and ordered channels, which can provide a large number of sites for the adsorption and ORR of O2. The H2O2 formation rate catalyzed by TPB-DMTP-COF was 2882μmol·g-1·h-1, which was 15 times higher than that of the two-phase reaction system, and the SCC efficiency reached 0.76%.

5 Conclusion and prospect

In this paper, the mechanism of photocatalytic generation of H2O2 and the reason for the low efficiency of H2O2 are discussed. The photocatalyst materials currently developed and utilized were introduced, including g-C3N4, a series of metal oxides and metal sulfides, and organic frameworks. The strategies to improve the photocatalytic generation of H2O2 are also highlighted, including morphology optimization, defect control, heterojunction engineering, supported metal nanoparticles, element doping, quantum dot modification, introduction of organic molecules or groups, and construction of three-phase reaction systems. At present, the H2O2 of photocatalytic production has been improved to millimolar level, but it is far from meeting the requirements of industrial production. The effective adsorption of O2, the effective utilization of visible light, the separation and transfer efficiency of e--h+ pairs, the optimization of H2O2 generation path and the rapid decomposition of generated H2O2 need to be further solved, and the stability of photocatalyst needs to be further improved. In addition, most photocatalytic systems use organic sacrificial agents, which consume h+ and inhibit the recombination of e--h+, but increase the reaction cost and make the subsequent purification of H2O2 difficult. In fact, most of the current research focuses on how to modify the photocatalyst materials, while neglecting the study of advanced photocatalytic systems or reactors.
Therefore, the generation efficiency and selectivity of photocatalytic H2O2 production need to be further improved. First, the absorption of visible light by the photocatalyst should be maximally expanded. The combination of defect engineering and other modification methods can be considered. It is impossible to improve the quality of AQE or AQY only by reducing the band gap of photocatalysis through defect engineering. It is necessary to further adjust the electronic structure and increase the adsorption sites of O2. Secondly, the decomposition of H2O2 should be inhibited while promoting the formation of H2O2, and the methods of loading metal NPs and doping elements can inhibit the adsorption of H2O2 on the surface of catalyst.So as to inhibit the decomposition of the H2O2, or to explore new methods for separating the generated H2O2 in time and inhibiting the decomposition of the H2O2. Finally, the kinetics of photocatalytic production of H2O2 was further studied to further understand the three pathways of photocatalytic production of H2O2. To understand the mechanism of e--h+ pair generation and recombination, and to explore ways to prolong the "life" of e--h+ pair. In addition, the generation of H2O2 by photocatalysis is coupled with the generation of organic matter, which may solve the problem of H2O2 decomposition to some extent. Although the technology of photocatalytic production of H2O2 is still in its infancy, it has great prospects for development, and more work needs to be done in the future. If the above aspects are addressed and improved, the photocatalytic production of H2O2 can be expected to be applied to industrial production and commercial applications.

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Funding

National Natural Science Foundation of China(22272034)

Guangdong Province Universities and Colleges Pearl River Scholar Funded Scheme of China(2019)

Guangdong Basic and Applied Basic Research Foundation(2021A1515010305)

Guangdong Basic and Applied Basic Research Foundation(2022A1515011900)

Environment and Energy Green Catalysis Innovation Team of Colleges and Universities of Guangdong Province(2022KCXTD019)

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